SIST EN ISO 11890-2:2014
(Main)Paints and varnishes - Determination of volatile organic compound (VOC) content - Part 2: Gas-chromatographic method (ISO 11890-2:2013)
Paints and varnishes - Determination of volatile organic compound (VOC) content - Part 2: Gas-chromatographic method (ISO 11890-2:2013)
This part of ISO 11890 is one of a series of standards dealing with the sampling and testing of paints, varnishes and related products. It specifies a method for the determination of the volatile organic compound (VOC) content of paints, varnishes and their raw materials. This part is preferred if the expected VOC content is greater than 0,1 % by mass and less than about 15 % by mass. When the VOC content is greater than about 15 % by mass, the less complicated method given in ISO 11890-1 may be used. This method assumes that the volatile matter is either water or organic. However, other volatile inorganic compounds can be present and might need to be quantified by another suitable method and allowed for in the calculations.
Beschichtungsstoffe - Bestimmung des Gehaltes an flüchtigen organischen Verbindungen (VOC-Gehalt) - Teil 2: Gaschromatographisches Verfahren (ISO 11890-2:2013)
Dieser Teil von ISO 11890 gehört zu einer Reihe von Normen, welche die Probenahme und Prüfung von Beschichtungsstoffen und ähnlichen Produkten behandelt.
Er legt ein Verfahren zum Bestimmen des Gehaltes an flüchtigen organischen Verbindungen (VOC-Gehalt) in Beschichtungsstoffen und deren Rohstoffen fest. Dieser Teil darf angewendet werden, wenn der erwartete VOC-Gehalt über 0,1 % (Massenanteil) und unter 15 % (Massenanteil) liegt. Wenn der VOC-Gehalt über 15 % (Massenanteil) liegt, sollte das weniger komplizierte Verfahren nach ISO 11890-1 angewendet werden.
Dieses Verfahren geht davon aus, dass es sich bei den flüchtigen Anteilen entweder um Wasser oder um organische Verbindungen handelt. Es können jedoch andere flüchtige anorganische Verbindungen anwesend sein, die durch ein anderes geeignetes Verfahren bestimmt und in den Berechnungen berücksichtigt werden dürfen.
Peintures et vernis - Détermination de la teneur en composés organiques volatils (COV) - Partie 2: Méthode par chromatographie en phase gazeuse (ISO 11890-2:2013)
L'ISO 11890-2:2013 fait partie d'une série de normes qui traitent de l'échantillonnage et des essais relatifs aux peintures, vernis et produits assimilés.
Elle spécifie une méthode de détermination de la teneur en composés organiques volatils (COV) des peintures, vernis et de leurs matières premières. Cette méthode est à utiliser de préférence si la teneur escomptée en COV est comprise entre 0,1 % en masse et environ 15 % en masse. Si la teneur en COV est supérieure à environ 15 % en masse, la méthode plus simple préconisée dans l'ISO 11890-1 peut être utilisée.
Cette méthode suppose que la matière volatile est de l'eau ou une matière organique. Toutefois, d'autres composés inorganiques volatils peuvent être présents; il pourrait être nécessaire de les quantifier selon une autre méthode et d'en tenir compte dans les calculs.
Barve in laki - Določevanje hlapnih organskih spojin (VOC) - 2. del: Metoda plinske kromatografije (ISO 11890-2:2013)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 11890-2:2014
01-februar-2014
1DGRPHãþD
SIST EN ISO 11890-2:2007
%DUYHLQODNL'RORþHYDQMHKODSQLKRUJDQVNLKVSRMLQ92&GHO0HWRGDSOLQVNH
NURPDWRJUDILMH,62
Paints and varnishes - Determination of volatile organic compound (VOC) content - Part
2: Gas-chromatographic method (ISO 11890-2:2013)
Beschichtungsstoffe - Bestimmung des Gehaltes an flüchtigen organischen
Verbindungen (VOC-Gehalt) - Teil 2: Gaschromatographisches Verfahren (ISO 11890-
2:2013)
Peintures et vernis - Détermination de la teneur en composés organiques volatils (COV)
- Partie 2: Méthode par chromatographie en phase gazeuse (ISO 11890-2:2013)
Ta slovenski standard je istoveten z: EN ISO 11890-2:2013
ICS:
87.040 Barve in laki Paints and varnishes
SIST EN ISO 11890-2:2014 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 11890-2:2014
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SIST EN ISO 11890-2:2014
EUROPEAN STANDARD
EN ISO 11890-2
NORME EUROPÉENNE
EUROPÄISCHE NORM
March 2013
ICS 87.040 Supersedes EN ISO 11890-2:2006
English Version
Paints and varnishes - Determination of volatile organic
compound (VOC) content - Part 2: Gas-chromatographic
method (ISO 11890-2:2013)
Peintures et vernis - Détermination de la teneur en Beschichtungsstoffe - Bestimmung des Gehaltes an
composés organiques volatils (COV) - Partie 2: Méthode flüchtigen organischen Verbindungen (VOC-Gehalt) - Teil
par chromatographie en phase gazeuse (ISO 11890- 2: Gaschromatographisches Verfahren (ISO 11890-2:2013)
2:2013)
This European Standard was approved by CEN on 28 February 2013.
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-CENELEC 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-CENELEC Management Centre has the same
status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United
Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2013 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 11890-2:2013: E
worldwide for CEN national Members.
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SIST EN ISO 11890-2:2014
EN ISO 11890-2:2013 (E)
Contents Page
Foreword .3
2
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SIST EN ISO 11890-2:2014
EN ISO 11890-2:2013 (E)
Foreword
This document (EN ISO 11890-2:2013) has been prepared by Technical Committee ISO/TC 35 "Paints and
varnishes" in collaboration with Technical Committee CEN/TC 139 “Paints and varnishes” the secretariat of
which is held by DIN.
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 September 2013, and conflicting national standards shall be
withdrawn at the latest by September 2013.
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 11890-2:2006.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech
Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece,
Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,
Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.
Endorsement notice
The text of ISO 11890-2:2013 has been approved by CEN as EN ISO 11890-2:2013 without any modification.
3
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SIST EN ISO 11890-2:2014
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SIST EN ISO 11890-2:2014
INTERNATIONAL ISO
STANDARD 11890-2
Third edition
2013-03-15
Paints and varnishes —
Determination of volatile organic
compound (VOC) content —
Part 2:
Gas-chromatographic method
Peintures et vernis — Détermination de la teneur en composés
organiques volatils (COV) —
Partie 2: Méthode par chromatographie en phase gazeuse
Reference number
ISO 11890-2:2013(E)
©
ISO 2013
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SIST EN ISO 11890-2:2014
ISO 11890-2:2013(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2013
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of
the requester.
ISO copyright office
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Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2013 – All rights reserved
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SIST EN ISO 11890-2:2014
ISO 11890-2:2013(E)
Contents Page
Foreword .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 2
5 Required supplementary information . 2
6 Apparatus . 2
6.1 Gas chromatograph . 2
6.2 Sample injection system . 3
6.3 Oven . 3
6.4 Detector . 3
6.5 Capillary column. 4
6.6 Qualitative-analysis equipment . 4
6.7 Injection syringe . 4
6.8 Chart recorder . 4
6.9 Integrator . 4
6.10 Sample vials . 4
6.11 Gas filters . 4
6.12 Gases . 4
7 Reagents . 5
7.1 Internal standard . 5
7.2 Calibration compounds . 5
7.3 Dilution solvent . 5
7.4 Marker compound . 5
8 Sampling . 5
9 Procedure. 5
9.1 Density . 5
9.2 Water content . 6
9.3 Gas-chromatographic conditions . 6
9.4 Qualitative analysis of product . 6
9.5 Calibration . 6
9.6 Sample preparation . 7
9.7 Quantitative determination of compound content . 7
10 Calculation . 8
10.1 General . 8
10.2 Method 1: VOC content, as a percentage by mass, of the product “ready for use” . 8
10.3 Method 2: VOC content, in grams per litre, of the product “ready for use” . 9
10.4 Method 3: VOC content, in grams per litre, of the product “ready for use” less water . 9
10.5 Method 4: VOC content, in grams per litre, of the product “ready for use” less water and
less exempt compounds (only required if national legislation applies) .10
11 Expression of results .10
12 Precision .10
12.1 General .10
12.2 Repeatability limit r . 10
12.3 Reproducibility limit R . 11
13 Test report .11
Annex A (normative) Required supplementary information .12
Annex B (informative) Examples of gas-chromatographic conditions .13
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SIST EN ISO 11890-2:2014
ISO 11890-2:2013(E)
Bibliography .17
iv © ISO 2013 – All rights reserved
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SIST EN ISO 11890-2:2014
ISO 11890-2:2013(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 11890-2 was prepared by Technical Committee ISO/TC 35, Paints and varnishes.
This third edition cancels and replaces the second edition (ISO 11890-2:2006), of which it constitutes a
minor revision to correct the numerator of the fraction in Equation (6) in 10.5.
ISO 11890 consists of the following parts, under the general title Paints and varnishes — Determination
of volatile organic compound (VOC) content:
— Part 1: Difference method
— Part 2: Gas-chromatographic method
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SIST EN ISO 11890-2:2014
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SIST EN ISO 11890-2:2014
INTERNATIONAL STANDARD ISO 11890-2:2013(E)
Paints and varnishes — Determination of volatile organic
compound (VOC) content —
Part 2:
Gas-chromatographic method
1 Scope
This part of ISO 11890 is one of a series of standards dealing with the sampling and testing of paints,
varnishes and related products.
It specifies a method for the determination of the volatile organic compound (VOC) content of paints,
varnishes and their raw materials. This part is preferred if the expected VOC content is greater than
0,1 % by mass and less than about 15 % by mass. When the VOC content is greater than about 15 % by
mass, the less complicated method given in ISO 11890-1 may be used.
This method assumes that the volatile matter is either water or organic. However, other volatile inorganic
compounds can be present and might need to be quantified by another suitable method and allowed for
in the calculations.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
ISO 760, Determination of water — Karl Fischer method (General method)
ISO 1513, Paints and varnishes — Examination and preparation of test samples
ISO 2811-1, Paints and varnishes — Determination of density — Part 1: Pyknometer method
ISO 2811-2, Paints and varnishes — Determination of density — Part 2: Immersed body (plummet) method
ISO 2811-3, Paints and varnishes — Determination of density — Part 3: Oscillation method
ISO 2811-4, Paints and varnishes — Determination of density — Part 4: Pressure cup method
ISO 15528, Paints, varnishes and raw materials for paints and varnishes — Sampling
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
volatile organic compound
VOC
any organic liquid and/or solid that evaporates spontaneously at the prevailing temperature and
pressure of the atmosphere with which it is in contact
Note 1 to entry: As to current usage of the term VOC in the field of coating materials, see volatile organic compound
content (VOC content).
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SIST EN ISO 11890-2:2014
ISO 11890-2:2013(E)
Note 2 to entry: Under US government legislation, the term VOC is restricted solely to those compounds that are
photochemically active in the atmosphere (see ASTM D3960). Any other compound is then defined as being an
exempt compound.
Note 3 to entry: Under European legislation, EU Directive 2004/42/EC, the term VOC refers to volatile organic
compounds with boiling points up to 250 °C, measured at a standard pressure of 101,3 kPa.
[SOURCE: ISO 4618:2006, modified — Note 3 to entry has been added.]
3.2
volatile organic compound content
VOC content
mass of the volatile organic compounds present in a coating material, as determined under specified
conditions
Note 1 to entry: The properties and the amounts of the compounds to be taken into account will depend on the
field of application of the coating material. For each field of application, the limiting values and the methods of
determination or calculation are stipulated by regulations or by agreement.
Note 2 to entry: If the term VOC refers to compounds with a defined maximum boiling point (see Note 3 to 3.1), the
compounds considered to be part of the VOC content are those with boiling points below that limit, and compounds
with higher boiling points are considered to be non-volatile organic compounds.
[SOURCE: ISO 4618:2006, modified — Note 2 to entry has been added.]
3.3
exempt compound
organic compound that does not participate in atmospheric photochemical reactions
Note 1 to entry: See Note 2 to entry and Note 3 to entry in 3.1)
3.4
ready for use
state of a product when it is mixed in accordance with the manufacturer’s instructions in the correct
proportions and thinned if required using the correct thinners so that it is ready for application by the
approved method
4 Principle
After preparation of the sample, the VOCs are separated by a gas-chromatographic technique. Either a
hot or a cold sample injection system is used, depending on the sample type. Hot injection is the preferred
method. After the compounds have been identified, they are quantified from the peak areas using an
internal standard. Depending on the equipment used, it might also be possible to determine the water
content by this method. A calculation is then performed to give the VOC content of the sample.
5 Required supplementary information
For any particular application, the test method specified in this part of ISO 11890 needs to be completed
by supplementary information. The items of supplementary information are given in Annex A.
6 Apparatus
6.1 Gas chromatograph
The apparatus shall be set up and used in accordance with the manufacturer’s instructions. All of the
instrumental parts coming into contact with the test sample shall be made of a material (e.g. glass)
which is resistant to the sample and will not change it chemically.
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SIST EN ISO 11890-2:2014
ISO 11890-2:2013(E)
6.2 Sample injection system
6.2.1 General
Use one of the two types specified in 6.2.2 and 6.2.3.
6.2.2 Hot-injection system with sample splitter (preferred system)
The instrument shall have a variable-temperature injection block with a sample splitter. The injection
temperature shall be capable of being set to an accuracy of 1 °C. The split ratio shall be adjustable and
capable of being monitored. The sample splitter insert shall contain silanized glass wool to retain non-
volatile constituents, and shall be cleaned and provided with new glass wool packing or replaced as
required to rule out errors due to residues of binder or pigment (i.e. adsorption of compounds). The
occurrence of adsorption is revealed by peak tailing, in particular with components of low volatility.
6.2.3 Cold-injection system with sample splitter
The cold-injection system shall be provided with temperature programming for heating from ambient
to 300 °C and shall have a sample splitter inlet which is made of an inert material such as glass. The
sample splitter shall be provided with silanized glass wool packing and shall be maintained as specified
in 6.2.2. The split ratio shall be adjustable and capable of being monitored.
Method precision will be increased if the injection system, especially the hot-injection system, is coupled
to an auto-injector. The manufacturer’s instructions shall be followed when an auto-injector is used.
6.2.4 Selection of sample injection system
The choice between hot-injection and cold-injection will depend on the type of product under test. It
will be necessary to use the cold-injection system for products which, at high temperature, release
substances which interfere with the determination.
Indications of cleavage or decomposition reactions can be obtained by looking for changes in the
chromatogram (for example the occurrence of foreign peaks or an increase or decrease in peak size) at
various sample injector temperatures.
The hot-injection system covers all of the volatile constituents, compounds and cleavage products of the
binders and additives. Cleavage products of the binders or additives which are identical to a constituent
of the product can be separated by a cold-injection system, since they elute later as a result of the
programmed increase in injection block temperature.
6.3 Oven
The oven shall be capable of being heated between 40 °C and 300 °C both isothermally and under
programmed temperature control. It shall be possible to set the oven temperature to within 1 °C. The
final temperature of the temperature programme shall not exceed the maximum operating temperature
of the column (see 6.5).
6.4 Detector
Any of the following three detectors may be used, as well as other detectors suitable for specific
types of compound:
6.4.1 Flame ionization detector (FID), capable of being operated at temperatures up to 300 °C.
To prevent condensation, the detector temperature shall be at least 10 °C above the maximum oven
temperature. The detector gas supply, injection volume, split ratio and gain setting shall be optimized so
that the signals (peak areas) used for the calculation are proportional to the amount of substance.
6.4.2 Suitably calibrated and tuned mass spectrometer or other mass-selective detector.
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SIST EN ISO 11890-2:2014
ISO 11890-2:2013(E)
6.4.3 Suitably calibrated Fourier-transform infrared spectrometer (FT-IR spectrometer).
6.5 Capillary column
The column shall be made of glass or fused silica. Columns of sufficient length to resolve volatiles
and of maximum internal diameter 0,32 mm, coated with unmodified or phenyl-modified
poly(dimethylsiloxane) or poly(ethylene glycol) at a suitable film thickness, have been shown to give
good peak separation. The stationary phase and column length shall be chosen to suit the particular
separation (see examples in Annex B).
A suitable combination of column, temperature programme and marker compound shall be chosen such
that compounds in the sample which are defined as VOCs by virtue of their boiling point (see Note 3 to
3.1) elute before the boiling-point marker compound (see 7.4) and those which are not VOCs elute after
the marker compound. When the boiling-point limit is set at 250 °C and a polar stationary phase is used,
1)
the marker compound given in 7.4, with a DB-1301™ column , or equivalent, at least 60 m in length and
with an internal diameter of 0,32 mm, and with a film thickness of approximately 1 µm, is recommended.
6.6 Qualitative-analysis equipment
If the separated components are to be identified by a mass-selective detector or FT-IR spectrometer,
the instrument shall be coupled to the gas chromatograph and operated in accordance with the
manufacturer’s instructions.
6.7 Injection syringe
The injection syringe shall have a capacity of at least twice the volume of the sample to be injected into
the gas chromatograph.
6.8 Chart recorder
Compensating chart recorders are suitable for plotting the gas chromatogram.
6.9 Integrator
An electronic data-processing system (integrator or computer) shall be used to measure the peak areas.
The integration parameters used in calibration and analysis shall be identical.
6.10 Sample vials
Use vials made of chemically inert material (e.g. glass) which can be sealed with a suitable septum cap
[e.g. a rubber membrane coated with poly(tetra fluoro ethylene)].
6.11 Gas filters
Filters shall be installed in the gas chromatograph connection pipes to adsorb residual impurities in the
gases (see 6.12).
6.12 Gases
6.12.1 Carrier gas: dry, oxygen-free helium, nitrogen or hydrogen, having a purity of at least
99,996 % by volume.
1) DB-1301 is the trademark of a product supplied by Agilent Technologies J&W. This information is given for the
convenience of users of this International Standard and does not constitute an endorsement by ISO of the product
named. Equivalent products may be used if they can be shown to lead to the same results.
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SIST EN ISO 11890-2:2014
ISO 11890-2:2013(E)
6.12.2 Detector gases: hydrogen having a purity of at least 99,999 % by volume and air (
...
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