ISO 11890-2:2020

Paints and varnishes — Determination of volatile organic compounds(VOC) and/or semi volatile organic compounds (SVOC) content — Part 2: Gas-chromatographic method

This document is applicable for the determination of VOC and SVOC with an expected VOC and/or SVOC content greater than 0,01 % by mass up to 100 % by mass. The method given in ISO 11890-1 is used when the VOC is greater than 15 % by mass. This document (method ISO 11890-2) applies when the system contains VOC and SVOC as the VOC result of ISO 11890-1 can be influenced by the SVOC. For VOC content smaller than 0,1 %, the head space method described in ISO 17895 is used as an alternative. ISO 11890-1 and ISO 17895 cannot be used for the determination of the SVOC content. NOTE 1 Some ingredients of coating materials and their raw materials can decompose during analysis and cause artificial VOC and/or SVOC signals. When determining VOC and/or SVOC for coating materials and their raw materials, these signals are artefacts of the method and are not taken into account (examples are given in Annex B). 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. The method defined in this document is not applicable for determination of water content. NOTE 2 If organic acids or bases and their corresponding salts are present in the coating material or its raw materials, the amount that is quantified by this method might not be accurate due to a change in the acid or base equilibrium.

Peintures et vernis — Détermination de la teneur en composés organiques volatils (COV) et/ou composés organiques semi-volatils (COSV) — Partie 2: Méthode par chromatographie en phase gazeuse

Le présent document est applicable à la détermination des COV et des COSV pour lesquels la teneur attendue en COV et/ou en COSV est supérieure à 0,01 % en masse et jusqu'à 100 % en masse. La méthode donnée dans l'ISO 11890-1 est utilisée lorsque la teneur en COV est supérieure à 15 % en masse. Le présent document (méthode ISO 11890-2) s'applique lorsque le système contient des COV et des COSV, car le résultat obtenu selon l'ISO 11890-1 peut être influencé par les COSV. Pour une teneur en COV inférieure à 0,1 %, la méthode de l'espace de tête décrite dans l'ISO 17895 est utilisée en guise d'alternative. L'ISO 11890-1 et l'ISO 17895 ne peuvent pas être utilisées pour la détermination de la teneur en COSV. NOTE 1 Certains ingrédients des produits de peinture et de leurs matières premières peuvent se décomposer pendant l'analyse et causer des signaux COV et/ou COSV artificiels. Lors de la détermination des COV et/ou des COSV dans les produits de peinture et leurs matières premières, ces signaux sont des artefacts de la méthode et ne sont pas pris en compte (des exemples sont donnés à l'Annexe B). 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 adaptée et d'en tenir compte dans les calculs. La méthode définie dans le présent document n'est pas applicable à la détermination de la teneur en eau. NOTE 2 Si des acides ou des bases organiques et leurs sels correspondants sont présents dans le produit de peinture ou ses matières premières, la quantité qui est quantifiée par cette méthode pourrait ne pas être exacte en raison d'une modification de l'équilibre acido-basique.

General Information

• Status: Published
• Publication Date: 22-Jun-2020
• ICS: 87.040 - Paints and varnishes
• Technical Committee: ISO/TC 35/SC 16 - Chemical analysis
• Drafting Committee: ISO/TC 35/SC 16/WG 1 - Volatile and semi-volatile organic compounds
• Parallel Committee: ISO/TC 28 - Petroleum and related products, fuels and lubricants from natural or synthetic sources
• Current Stage: 6060 - International Standard published
• Start Date: 23-Jun-2020
• Due Date: 29-Feb-2020
• Completion Date: 23-Jun-2020

Relations

• Revises: ISO 11890-2:2013 - Paints and varnishes — Determination of volatile organic compound (VOC) content — Part 2: Gas-chromatographic method
• Effective Date: 10-Dec-2016

Standards Content (Sample)

INTERNATIONAL ISO
STANDARD 11890-2
Fourth edition
2020-06
Paints and varnishes — Determination
of volatile organic compounds(VOC)
and/or semi volatile organic
compounds (SVOC) content —
Part 2:
Gas-chromatographic method
Peintures et vernis — Détermination de la teneur en composés
organiques volatils (COV) et/ou composés organiques semi-volatils
(COSV) —
Partie 2: Méthode par chromatographie en phase gazeuse
Reference number
ISO 11890-2:2020(E)
ISO 2020
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ISO 11890-2:2020(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2020

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting

on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address

below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: [phone]
Email: [e-mail]
Website: www.iso.org
Published in Switzerland
ii © ISO 2020 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 11890-2:2020(E)
Contents Page

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

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

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

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

3 Terms and definitions ..................................................................................................................................................................................... 2

4 Principle ........................................................................................................................................................................................................................ 4

5 Required information ..................................................................................................................................................................................... 4

6 Apparatus ..................................................................................................................................................................................................................... 4

7 Reagents ........................................................................................................................................................................................................................ 7

8 Procedure..................................................................................................................................................................................................................... 8

8.1 Sampling ....................................................................................................................................................................................................... 8

8.2 Analysis.......................................................................................................................................................................................................... 8

8.2.1 Sample preparation ....................................................................................................................................................... 8

8.2.2 Data acquisition for sample measurement ............................................................................................... 8

8.3 Calibration .................................................................................................................................................................................................. 9

8.3.1 General...................................................................................................................................................................................... 9

8.3.2 Preparation of calibration solutions ............................................................................................................... 9

8.3.3 Analysis of the multi-point calibration ......................................................................................................... 9

8.4 Quality assurance...............................................................................................................................................................................10

8.5 Gas chromatographic conditions ..........................................................................................................................................10

8.6 Density ........................................................................................................................................................................................................10

8.7 Water content ........................................................................................................................................................................................10

9 Data analysis ..........................................................................................................................................................................................................11

9.1 Integration and identification of compounds ............................................................................................................11

9.2 Classification of compounds .....................................................................................................................................................13

10 Quantitative determination of compound content ........................................................................................................15

10.1 General ........................................................................................................................................................................................................15

10.2 Quantitative determination of compound content ...............................................................................................17

10.2.1 Quantification with respect to CSRF ............................................................................................................17

10.2.2 Quantification with respect to surrogate standard .........................................................................17

11 Calculation of VOC and SVOC content ...........................................................................................................................................17

11.1 General ........................................................................................................................................................................................................17

11.2 Method 1 — VOC content and/or SVOC content, as a percentage by mass, of the

product “ready for use” .................................................................................................................................................................18

11.3 Method 2 — VOC content and/or SVOC content, in grams per litre, of the product

“ready for use” ......................................................................................................................................................................................18

11.4 Method 3 — VOC content and/or SVOC content, in grams per litre, of the product

“ready for use” less water ...........................................................................................................................................................19

11.5 Method 4 — VOC content and/or SVOC content, in grams per litre, of the product

“ready for use” less water and less exempt compounds .................................................................................19

12 Data evaluation and calculation of final results ...............................................................................................................20

13 Precision ....................................................................................................................................................................................................................21

13.1 General ........................................................................................................................................................................................................21

13.2 Repeatability limit, r ......................................................................................................................................................................21

13.3 Reproducibility limit, R ................................................................................................................................................................21

14 Test report ................................................................................................................................................................................................................21

Annex A (normative) Non-exhaustive list of VOC, SVOC and NVOC compounds ...................................................22

© ISO 2020 – All rights reserved iii
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ISO 11890-2:2020(E)

Annex B (informative) Information on thermal unstable products ..................................................................................28

Annex C (informative) Examples for GC method conditions .....................................................................................................35

Annex D (informative) Results of the round robin test for the determination of precision data.......37

Bibliography .............................................................................................................................................................................................................................39

iv © ISO 2020 – All rights reserved
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ISO 11890-2:2020(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.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of

any patent rights identified during the development of the document will be in the Introduction and/or

on the ISO list of patent declarations received (see www .iso .org/ patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO's adherence to the

World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see www .iso .org/

iso/ foreword .html.

This document was prepared by Technical Committee ISO/TC 35, Paints and varnishes, in collaboration

with the European Committee for Standardization (CEN) Technical Committee CEN/TC 139, Paints and

varnishes, in accordance with the Agreement on technical cooperation between ISO and CEN (Vienna

Agreement).

This fourth edition cancels and replaces the third edition (ISO 11890-2:2013), which has been

technically revised.
The main changes compared to the previous edition are as follows:

— the scope has been expanded to include the determination of semi volatile organic compounds (SVOC);

— the scope has been expanded to include concentration ranges from 0,01 % to 100 %;

— the specifications for determination of semi-volatile organic compounds have been added.

A list of all parts in the ISO 11890 series can be found on the ISO website.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www .iso .org/ members .html.
© ISO 2020 – All rights reserved v
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ISO 11890-2:2020(E)
Introduction

This document is one of a series of standards dealing with the sampling and testing of coating materials

and their raw materials. It specifies a method for the determination of the volatile organic compounds

(VOC) content and the semi-volatile organic compounds (SVOC) content of coating materials and their

raw materials.
vi © ISO 2020 – All rights reserved
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INTERNATIONAL STANDARD ISO 11890-2:2020(E)
Paints and varnishes — Determination of volatile organic
compounds(VOC) and/or semi volatile organic compounds
(SVOC) content —
Part 2:
Gas-chromatographic method

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

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

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

to ensure the safety and health of personnel prior to the application of the document, and to

determine the applicability of any other restrictions for this purpose.
1 Scope

This document is applicable for the determination of VOC and SVOC with an expected VOC and/or SVOC

content greater than 0,01 % by mass up to 100 % by mass.

The method given in ISO 11890-1 is used when the VOC is greater than 15 % by mass. This document

(method ISO 11890-2) applies when the system contains VOC and SVOC as the VOC result of ISO 11890-1

can be influenced by the SVOC. For VOC content smaller than 0,1 %, the head space method described in

ISO 17895 is used as an alternative. ISO 11890-1 and ISO 17895 cannot be used for the determination of

the SVOC content.

NOTE 1 Some ingredients of coating materials and their raw materials can decompose during analysis and

cause artificial VOC and/or SVOC signals. When determining VOC and/or SVOC for coating materials and their

raw materials, these signals are artefacts of the method and are not taken into account (examples are given in

Annex B).

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. The method defined in this document is not applicable for determination

of water content.

NOTE 2 If organic acids or bases and their corresponding salts are present in the coating material or its raw

materials, the amount that is quantified by this method might not be accurate due to a change in the acid or base

equilibrium.
2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements 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 760, Determination of water — Karl Fischer method (General method)
ISO 1513, Paints and varnishes — Examination and preparation of test samples
ISO 2811 (all parts), Paints and varnishes — Determination of density

ISO 15528, Paints, varnishes and raw materials for paints and varnishes — Sampling

© ISO 2020 – All rights reserved 1
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ISO 11890-2:2020(E)
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

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

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

compounds content (VOC content) (3.4).

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 (3.6).
[SOURCE: ISO 4618:2014, 2.270]
3.2
semi-volatile organic compound
SVOC

organic liquid and/or solid that evaporates spontaneously but slower in comparison to VOC 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 SVOC in the field of coating materials, see semi-volatile organic

compounds content (SVOC content) (3.5).
3.3
non-volatile organic compound
NVOC
organic liquid and/or solid not classified as VOC or SVOC
3.4
volatile organic compounds content
VOC content
VOCC

mass of the volatile organic compounds (3.1) 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, the compounds

considered to be part of the VOC content are those with boiling points below and including that limit, and

compounds with higher boiling points are considered to be semi-volatile or non-volatile organic compounds.

[SOURCE: ISO 4618:2014, 2.271, modified — Note 2 to entry has been added.]
2 © ISO 2020 – All rights reserved
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ISO 11890-2:2020(E)
3.5
semi-volatile organic compounds content
SVOC content
SVOCC

mass of the semi-volatile organic compounds (3.2) 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 SVOC refers to compounds with a defined maximum boiling point and minimum

boiling point, the compounds considered to be part of the SVOC content are those with boiling points below and

including the upper and above the lower limit, and compounds with higher boiling points are considered to be

non-volatile organic compounds.
3.6
exempt compound

organic compound that does not participate in atmospheric photochemical reactions

Note 1 to entry: This expression is only relevant in some countries.
3.7
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
3.8
internal standard

compound which is not present in the sample, is completely separated from the other components in

the chromatogram, is inert with respect to the sample constituents, stable in the required temperature

range and of known purity and which is added to the sample to control the dilution and the injection

step of the analysis
3.9
surrogate standard
compound of known purity which is used to quantify unidentified VOCs and SVOCs
3.10
marker compound

compound which is used to differentiate between VOC and SVOC, or SVOC and NVOC if the differentiation

has to be made on the basis of retention time (3.11)
3.11
retention time

time elapsed from injection of the sample component to the recording of the peak maximum

3.12
extraction solvent
liquid used to extract the VOCs and SVOCs from the matrix under investigation
3.13
major peak
peak that contributes significantly to either

— the VOC content, i.e. ≥ 10 % of the absolute VOC content (as DEA equivalent) and ≥ 0,1 % by mass (as

DEA equivalent), or

— the SVOC content, i.e. ≥ 10 % of the absolute SVOC content (as DEA equivalent) and ≥ 0,1 % by mass

(as DEA equivalent)
© ISO 2020 – All rights reserved 3
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ISO 11890-2:2020(E)
3.14
minor peak
peak that contributes only to a minor extent to either

— the VOC content, i.e. < 0,1 % by mass (as DEA equivalent) and/or < 10 % of the absolute VOC content

(as DEA equivalent), or

— the SVOC content, i.e. < 0,1 % by mass (as DEA equivalent) and/or < 10 % of the absolute SVOC

content (as DEA equivalent)
3.15
reagent
substance used in chemical/biochemical analysis or other reactions
[SOURCE: ISO 20391-1:2018, 3.19]
4 Principle

After preparation of the sample, the VOCs, SVOCs and NVOCs 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, e.g. via GC-MS, they are

quantified from the peak areas with respect to their compound specific relative response with the

help of an internal standard, via GC-FID. Non-identifiable substances are quantified with respect to a

surrogate standard that can be identical to the internal standard. A calculation is performed to give the

VOC and/or SVOC content of the sample.
5 Required information

For any particular application, the information required should preferably be agreed between the

interested parties and may be derived, in part or totally, from an international or national standard or

other document related to the product under test.
The required information can include the following points:
a) the organic compound(s) to be determined (see Clause 9);
b) the experimental conditions to be used (see 8.5);
c) the classification criteria for VOC and/or SVOC;
d) which of the organic compounds in a) are exempt compounds (if relevant);
e) the method of calculation to be used (see Clause 10 and Clause 11).
6 Apparatus
6.1 Gas chromatograph

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.
Use one of the two types specified in 6.1.1 and 6.1.2.
4 © ISO 2020 – All rights reserved
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ISO 11890-2:2020(E)
6.1.1 Hot-injection system (preferred system)

The instrument shall have a variable-temperature injection block with sample splitter. The injection

temperature shall be capable of being set to an accuracy of 1 °C. Standard operating temperature shall

be between 250 °C and 280 °C.

NOTE It is useful to use silanized glass wool to retain non-volatile constituents. The active sides of silanized

glass wool can be a sink for organic compounds and significantly influence the recovery rate in the lower range

of the method. The occurrence of adsorption is revealed by peak tailing, in particular with components of low

volatility and/or high polarity.
6.1.2 Cold-injection system (programmed temperature vaporizer, PTV)

The cold-injection system shall be provided with temperature programming for heating from ambient

to 300 °C including a sample splitter for split operation.

NOTE It is useful to use silanized glass wool to retain non-volatile constituents. The active sides of silanized

glass wool can be a sink for organic compounds and significantly influence the recovery rate in the lower range

of the method. The occurrence of adsorption is revealed by peak tailing, in particular with components of low

volatility and/or high polarity.
6.1.3 Selection of sample injection system

The choice between hot-injection and cold-injection will depend on the type of product under test. It is

preferred to use the cold-injection system for products which, at high temperature, release substances

which interfere with the determination. Cleavage products of binders or additives can be reduced by

the use of cold injection system.

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 (see Annex B).
6.2 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 capillary column (see 6.4).
6.3 Detector
The following two detectors shall be used.

6.3.1 Mass spectrometer or other mass-selective detector (MS or MSD), for the identification of

VOC and SVOC compounds. To prevent condensation, the detector temperature shall be at least 10 °C

above the maximum oven temperature.

6.3.2 Flame ionization detector (FID), for quantification of VOC and SVOC compounds operated at

temperatures between 230 °C and 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.
© ISO 2020 – All rights reserved 5
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ISO 11890-2:2020(E)
6.4 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 5 % phenyl-modified poly(dimethylsiloxane) or 6 %

(cyanopropyl-phenyl)-methylpolysiloxane at a suitable film thickness shall be used.

NOTE Columns such as DB-5, HP-5, or DB-1301 are suitable . DB-5, HP-5 or DB-1301 are GC columns

characterized as equivalent to USP phase G27 or G43. Other columns equivalent USP phase G27 or G43, which

meet the pre-set performance criteria of this method can be used as well.
6.5 Analytical system performance criteria

The analytical system performance criteria shall be demonstrated. The limit of quantification (LOQ)

for the VOC content and SVOC content, respectively, is 0,01 % by mass. For single compounds, the LOQ

is assumed to be 0,005 % by mass using the response factor for diethyladipate (i.e. in DEA equivalents).

NOTE The limit of quantification can deviate for single compounds. If necessary, the compound specific limit

of quantification can be determined for the considered single compound(s).

Chromatographic resolution shall be sufficient to separate the compounds DEA and tetradecane (C14),

as well as docosane (C22) and dibutylsebacate (DBS). At least a resolution of 1 shall be reached.

For the quantification of VOC content and/or SVOC content at concentrations below 0,1 % by mass the LOQ

of triethylene glycol (TEG) shall be proven to be at least 0,005 % by mass, based on the sample weight.

6.6 Qualitative-analysis equipment

If the separated components are to be identified by a mass-selective detector, the instrument shall be

coupled to the gas chromatograph.
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 Data processing

A suitable software shall be used for integration, calibration, quantification and other data handling

processes.
6.9 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)].
6.10 Gas filters

Filters shall be installed in the gas chromatograph connection pipes to adsorb residual impurities in the

gases (6.11).
6.11 Gases

6.11.1 Carrier gas, dry, oxygen-free helium, nitrogen or hydrogen, having a purity of at least 99,996 %

by volume.

1) DB-5, HP-5 and DB-1301 are the trade names of products. This information is given for the convenience of users

of this document and
...

FINAL
INTERNATIONAL ISO/FDIS
DRAFT
STANDARD 11890-2
ISO/TC 35
Paints and varnishes — Determination
Secretariat: NEN
of volatile organic compounds(VOC)
Voting begins on:
2020-03-02 and/or semi volatile organic
compounds (SVOC) content —
Voting terminates on:
2020-04-27
Part 2:
Gas-chromatographic method
Peintures et vernis — Détermination de la teneur en composés
organiques volatils (COV) et composés organiques semi-volatils
(COSV) —
Partie 2: Méthode par chromatographie en phase gazeuse
Member bodies are requested to consult relevant national interests in ISO/TC
28 before casting their ballot to the e-Balloting application.
ISO/CEN PARALLEL PROCESSING
RECIPIENTS OF THIS DRAFT ARE INVITED TO
SUBMIT, WITH THEIR COMMENTS, NOTIFICATION
OF ANY RELEVANT PATENT RIGHTS OF WHICH
THEY ARE AWARE AND TO PROVIDE SUPPOR TING
DOCUMENTATION.
IN ADDITION TO THEIR EVALUATION AS
Reference number
BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO-
ISO/FDIS 11890-2:2020(E)
LOGICAL, COMMERCIAL AND USER PURPOSES,
DRAFT INTERNATIONAL STANDARDS MAY ON
OCCASION HAVE TO BE CONSIDERED IN THE
LIGHT OF THEIR POTENTIAL TO BECOME STAN-
DARDS TO WHICH REFERENCE MAY BE MADE IN
NATIONAL REGULATIONS. ISO 2020
---------------------- Page: 1 ----------------------
ISO/FDIS 11890-2:2020(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2020

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting

on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address

below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: [phone]
Fax: [phone]
Email: [e-mail]
Website: www.iso.org
Published in Switzerland
ii © ISO 2020 – All rights reserved
---------------------- Page: 2 ----------------------
ISO/FDIS 11890-2:2020(E)
Contents Page

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

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

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

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

3 Terms and definitions ..................................................................................................................................................................................... 2

4 Principle ........................................................................................................................................................................................................................ 4

5 Required information ..................................................................................................................................................................................... 4

6 Apparatus ..................................................................................................................................................................................................................... 4

7 Reagents ........................................................................................................................................................................................................................ 7

8 Procedure..................................................................................................................................................................................................................... 8

8.1 Sampling ....................................................................................................................................................................................................... 8

8.2 Analysis.......................................................................................................................................................................................................... 8

8.2.1 Sample preparation ....................................................................................................................................................... 8

8.2.2 Data acquisition for sample measurement ............................................................................................... 8

8.3 Calibration .................................................................................................................................................................................................. 9

8.3.1 General...................................................................................................................................................................................... 9

8.3.2 Preparation of calibration solutions ............................................................................................................... 9

8.3.3 Analysis of the multi-point calibration ......................................................................................................... 9

8.4 Quality assurance...............................................................................................................................................................................10

8.5 Gas chromatographic conditions ..........................................................................................................................................10

8.6 Density ........................................................................................................................................................................................................10

8.7 Water content ........................................................................................................................................................................................10

9 Data analysis ..........................................................................................................................................................................................................11

9.1 Integration and identification of compounds ............................................................................................................11

9.2 Classification of compounds .....................................................................................................................................................13

10 Quantitative determination of compound content ........................................................................................................15

10.1 General ........................................................................................................................................................................................................15

10.2 Quantitative determination of compound content ...............................................................................................17

10.2.1 Quantification with respect to CSRF ............................................................................................................17

10.2.2 Quantification with respect to surrogate standard .........................................................................17

11 Calculation of VOC and SVOC content ...........................................................................................................................................17

11.1 General ........................................................................................................................................................................................................17

11.2 Method 1 — VOC content and/or SVOC content, as a percentage by mass, of the

product “ready for use” .................................................................................................................................................................18

11.3 Method 2 — VOC content and/or SVOC content, in grams per litre, of the product

“ready for use” ......................................................................................................................................................................................18

11.4 Method 3 — VOC content and/or SVOC content, in grams per litre, of the product

“ready for use” less water ...........................................................................................................................................................19

11.5 Method 4 — VOC content and/or SVOC content, in grams per litre, of the product

“ready for use” less water and less exempt compounds .................................................................................19

12 Data evaluation and calculation of final results ...............................................................................................................20

13 Precision ....................................................................................................................................................................................................................20

13.1 General ........................................................................................................................................................................................................20

13.2 Repeatability limit, r ......................................................................................................................................................................21

13.3 Reproducibility limit, R ................................................................................................................................................................21

14 Test report ................................................................................................................................................................................................................21

Annex A (normative) Non-exhaustive list of VOC, SVOC and NVOC compounds ...................................................22

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ISO/FDIS 11890-2:2020(E)

Annex B (informative) Information on thermal unstable products ..................................................................................28

Annex C (informative) Examples for GC method conditions .....................................................................................................35

Annex D (informative) Results of the round robin test for the determination of precision data.......37

Bibliography .............................................................................................................................................................................................................................39

iv © ISO 2020 – All rights reserved
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ISO/FDIS 11890-2:2020(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.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of

any patent rights identified during the development of the document will be in the Introduction and/or

on the ISO list of patent declarations received (see www .iso .org/ patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO's adherence to the

World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see www .iso .org/

iso/ foreword .html.

This document was prepared by Technical Committee ISO/TC 35, Paints and varnishes, in collaboration

with the European Committee for Standardization (CEN) Technical Committee CEN/TC 139, Paints and

varnishes, in accordance with the Agreement on technical cooperation between ISO and CEN (Vienna

Agreement).

This fourth edition cancels and replaces the third edition (ISO 11890-2:2013), which has been

technically revised.
The main changes compared to the previous edition are as follows:

— the scope has been expanded to include the determination of semi volatile organic compounds (SVOC);

— the scope has been expanded to include concentration ranges from 0,01 % to 100 %;

— the specifications for determination of semi-volatile organic compounds have been added.

A list of all parts in the ISO 11890 series can be found on the ISO website.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www .iso .org/ members .html.
© ISO 2020 – All rights reserved v
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ISO/FDIS 11890-2:2020(E)
Introduction

This document is one of a series of standards dealing with the sampling and testing of coating materials

and their raw materials. It specifies a method for the determination of the volatile organic compounds

(VOC) content and the semi-volatile organic compounds (SVOC) content of coating materials and their

raw materials.
vi © ISO 2020 – All rights reserved
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FINAL DRAFT INTERNATIONAL STANDARD ISO/FDIS 11890-2:2020(E)
Paints and varnishes — Determination of volatile organic
compounds(VOC) and/or semi volatile organic compounds
(SVOC) content —
Part 2:
Gas-chromatographic method

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

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

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

to ensure the safety and health of personnel prior to the application of the document, and to

determine the applicability of any other restrictions for this purpose.
1 Scope

This document is applicable for the determination of VOC and SVOC with an expected VOC and/or SVOC

content greater than 0,01 % by mass up to 100 % by mass.

The method given in ISO 11890-1 is used when the VOC is greater than 15 % by mass. This document

(method ISO 11890-2) applies when the system contains VOC and SVOC as the VOC result of ISO 11890-1

can be influenced by the SVOC. For VOC content smaller than 0,1 %, the head space method described in

ISO 17895 is used as an alternative. ISO 11890-1 and ISO 17895 cannot be used for the determination of

the SVOC content.

NOTE 1 Some ingredients of coating materials and their raw materials can decompose during analysis and

cause artificial VOC and SVOC signals. When determining VOC and SVOC for coating materials and their raw

materials, these signals are artefacts of the method and are not taken into account (examples are given in

Annex B).

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. The method defined in this document is not applicable for determination

of water content.

NOTE 2 If organic acids or bases and their corresponding salts are present in the coating material or its raw

materials, the amount that is quantified by this method might not be accurate due to a change in the acid or base

equilibrium.
2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements 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 760, Determination of water — Karl Fischer method (General method)
ISO 1513, Paints and varnishes — Examination and preparation of test samples
ISO 2811 (all parts), Paints and varnishes — Determination of density

ISO 15528, Paints, varnishes and raw materials for paints and varnishes — Sampling

© ISO 2020 – All rights reserved 1
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ISO/FDIS 11890-2:2020(E)
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

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

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

compounds content (VOC content) (3.4).

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 (3.6).
[SOURCE: ISO 4618:2014, 2.270]
3.2
semi-volatile organic compound
SVOC

organic liquid and/or solid that evaporates spontaneously but slower in comparison to VOC 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 SVOC in the field of coating materials, see semi-volatile organic

compounds content (SVOC content) (3.5).
3.3
non-volatile organic compound
NVOC
organic liquid and/or solid not classified as VOC or SVOC
3.4
volatile organic compounds content
VOC content
VOCC

mass of the volatile organic compounds (3.1) 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, the compounds

considered to be part of the VOC content are those with boiling points below and including that limit, and

compounds with higher boiling points are considered to be semi-volatile or non-volatile organic compounds.

[SOURCE: ISO 4618:2014, 2.271, modified — Note 2 to entry has been added.]
2 © ISO 2020 – All rights reserved
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ISO/FDIS 11890-2:2020(E)
3.5
semi-volatile organic compounds content
SVOC content
SVOCC

mass of the semi-volatile organic compounds (3.2) 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 SVOC refers to compounds with a defined maximum boiling point and minimum

boiling point, the compounds considered to be part of the SVOC content are those with boiling points below and

including the upper and above the lower limit, and compounds with higher boiling points are considered to be

non-volatile organic compounds.
3.6
exempt compound

organic compound that does not participate in atmospheric photochemical reactions

Note 1 to entry: This expression is only relevant in some countries.
3.7
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
3.8
internal standard

compound which is not present in the sample, is completely separated from the other components in

the chromatogram, is inert with respect to the sample constituents, stable in the required temperature

range and of known purity and which is added to the sample to control the dilution and the injection

step of the analysis
3.9
surrogate standard
compound of known purity which is used to quantify unidentified VOCs and SVOCs
3.10
marker compound

compound which is used to differentiate between VOC and SVOC, or SVOC and NVOC if the differentiation

has to be made on the basis of retention time (3.11)
3.11
retention time

time elapsed from injection of the sample component to the recording of the peak maximum

3.12
extraction solvent
liquid used to extract the VOCs and SVOCs from the matrix under investigation
3.13
major peak
peak that contributes significantly to either

— the VOC content, i.e. ≥ 10 % of the absolute VOC content (as DEA equivalent) and ≥ 0,1 % by mass (as

DEA equivalent), or

— the SVOC content, i.e. ≥ 10 % of the absolute SVOC content (as DEA equivalent) and ≥ 0,1 % by mass

(as DEA equivalent)
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ISO/FDIS 11890-2:2020(E)
3.14
minor peak
peak that contributes only to a minor extent to either

— the VOC content, i.e. < 0,1 % by mass (as DEA equivalent) and/or < 10 % of the absolute VOC content

(as DEA equivalent), or

— the SVOC content, i.e. < 0,1 % by mass (as DEA equivalent) and/or < 10 % of the absolute SVOC

content (as DEA equivalent)
3.15
reagent
substance used in chemical/biochemical analysis or other reactions
[SOURCE: ISO 20391-1:2018, 3.19]
4 Principle

After preparation of the sample, the VOCs, SVOCs and NVOCs 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, e.g. via GC-MS, they are

quantified from the peak areas with respect to their compound specific relative response with the

help of an internal standard, via GC-FID. Non-identifiable substances are quantified with respect to a

surrogate standard that can be identical to the internal standard. A calculation is performed to give the

VOC and/or SVOC content of the sample.
5 Required information

For any particular application, the information required should preferably be agreed between the

interested parties and may be derived, in part or totally, from an international or national standard or

other document related to the product under test.
The required information can include the following points:
a) the organic compound(s) to be determined (see Clause 9);
b) the experimental conditions to be used (see 8.5);
c) the classification criteria for VOC and/or SVOC;
d) which of the organic compounds in a) are exempt compounds (if relevant);
e) the method of calculation to be used (see Clause 10 and Clause 11).
6 Apparatus
6.1 Gas chromatograph

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.
Use one of the two types specified in 6.1.1 and 6.1.2.
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ISO/FDIS 11890-2:2020(E)
6.1.1 Hot-injection system (preferred system)

The instrument shall have a variable-temperature injection block with sample splitter. The injection

temperature shall be capable of being set to an accuracy of 1 °C. Standard operating temperature shall

be between 250 °C and 280 °C.

NOTE It is useful to use silanized glass wool to retain non-volatile constituents. The active sides of silanized

glass wool can be a sink for organic compounds and significantly influence the recovery rate in the lower range

of the method. The occurrence of adsorption is revealed by peak tailing, in particular with components of low

volatility and/or high polarity.
6.1.2 Cold-injection system (programmed temperature vaporizer, PTV)

The cold-injection system shall be provided with temperature programming for heating from ambient

to 300 °C including a sample splitter for split operation.

NOTE It is useful to use silanized glass wool to retain non-volatile constituents. The active sides of silanized

glass wool can be a sink for organic compounds and significantly influence the recovery rate in the lower range

of the method. The occurrence of adsorption is revealed by peak tailing, in particular with components of low

volatility and/or high polarity.
6.1.3 Selection of sample injection system

The choice between hot-injection and cold-injection will depend on the type of product under test. It is

preferred to use the cold-injection system for products which, at high temperature, release substances

which interfere with the determination. Cleavage products of binders or additives can be reduced by

the use of cold injection system.

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 (see Annex B).
6.2 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 capillary column (see 6.4).
6.3 Detector
The following two detectors shall be used.

6.3.1 Mass spectrometer or other mass-selective detector (MS or MSD), for the identification of

VOC and SVOC compounds. To prevent condensation, the detector temperature shall be at least 10 °C

above the maximum oven temperature.

6.3.2 Flame ionization detector (FID), for quantification of VOC and SVOC compounds operated at

temperatures between 230 °C and 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.
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ISO/FDIS 11890-2:2020(E)
6.4 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 5 % phenyl-modified poly(dimethylsiloxane) or 6 %

(cyanopropyl-phenyl)-methylpolysiloxane at a suitable film thickness shall be used.

NOTE Columns such as DB-5, HP-5, or DB-1301 are suitable . DB-5, HP-5 or DB-1301 are GC columns

characterized as equivalent to USP phase G27 or G43. Other columns equivalent USP phase G27 or G43, which

meet the pre-set performance criteria of this method can be used as well.
6.5 Analytical system performance criteria

The analytical system performance criteria shall be demonstrated. The limit of quantification (LOQ)

for the VOC content and SVOC content, respectively, is 0,01 % by mass. For single compounds, the LOQ

is assumed to be 0,005 % by mass using the response factor for diethyladipate (i.e. in DEA equivalents).

NOTE The limit of quantification can deviate for single compounds. If necessary, the compound specific limit

of quantification can be determined for the considered single compound(s).

Chromatographic resolution shall be sufficient to separate the compounds DEA and tetradecane (C14),

as well as docosane (C22) and dibutylsebacate (DBS). At least a resolution of 1 shall be reached.

For the quantification of VOC content and/or SVOC content at concentrations below 0,1 % by mass the LOQ

of triethylene glycol (TEG) shall be proven to be at least 0,005 % by mass, based on the sample weight.

6.6 Qualitative-analysis equipment

If the separated components are to be identified by a mass-selective detector, the instrument shall be

coupled to the gas chromatograph.
6.7 Injection syringe
The injection syringe shall have a ca
...

NORME ISO
INTERNATIONALE 11890-2
Quatrième édition
2020-06
Peintures et vernis — Détermination
de la teneur en composés organiques
volatils (COV) et/ou composés
organiques semi-volatils (COSV) —
Partie 2:
Méthode par chromatographie en
phase gazeuse
Paints and varnishes — Determination of volatile organic
compounds(VOC) and/or semi volatile organic compounds (SVOC)
content —
Part 2: Gas-chromatographic method
Numéro de référence
ISO 11890-2:2020(F)
ISO 2020
---------------------- Page: 1 ----------------------
ISO 11890-2:2020(F)
DOCUMENT PROTÉGÉ PAR COPYRIGHT
© ISO 2020

Tous droits réservés. Sauf prescription différente ou nécessité dans le contexte de sa mise en œuvre, aucune partie de cette

publication ne peut être reproduite ni utilisée sous quelque forme que ce soit et par aucun procédé, électronique ou mécanique,

y compris la photocopie, ou la diffusion sur l’internet ou sur un intranet, sans autorisation écrite préalable. Une autorisation peut

être demandée à l’ISO à l’adresse ci-après ou au comité membre de l’ISO dans le pays du demandeur.

ISO copyright office
Case postale 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Genève
Tél.: [phone]
E-mail: [e-mail]
Web: www.iso.org
Publié en Suisse
ii © ISO 2020 – Tous droits réservés
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ISO 11890-2:2020(F)
Sommaire Page

Avant-propos ................................................................................................................................................................................................................................v

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

1 Domaine d’application ................................................................................................................................................................................... 1

2 Références normatives ................................................................................................................................................................................... 1

3 Termes et définitions ....................................................................................................................................................................................... 2

4 Principe .......................................................................................................................................................................................................................... 4

5 Informations requises .................................................................................................................................................................................... 4

6 Appareillage .............................................................................................................................................................................................................. 4

7 Réactifs ........................................................................................................................................................................................................................... 7

8 Mode opératoire.................................................................................................................................................................................................... 8

8.1 Échantillonnage ...................................................................................................................................................................................... 8

8.2 Analyse ........................................................................................................................................................................................................... 8

8.2.1 Préparation de l’échantillon ................................................................................................................................... 8

8.2.2 Acquisition de données pour le mesurage de l’échantillon ........................................................ 9

8.3 Étalonnage .................................................................................................................................................................................................. 9

8.3.1 Généralités ............................................................................................................................................................................ 9

8.3.2 Préparation des solutions d’étalonnage ...................................................................................................... 9

8.3.3 Analyse de l’étalonnage multipoint ................................................................................................................. 9

8.4 Assurance qualité...............................................................................................................................................................................11

8.5 Conditions de chromatographie en phase gazeuse ..............................................................................................11

8.6 Masse volumique................................................................................................................................................................................11

8.7 Teneur en eau ........................................................................................................................................................................................11

9 Analyse des données......................................................................................................................................................................................11

9.1 Intégration et identification des composés .................................................................................................................11

9.2 Classification des composés .....................................................................................................................................................14

10 Détermination quantitative de la teneur en composés .............................................................................................16

10.1 Généralités ...............................................................................................................................................................................................16

10.2 Détermination quantitative de la teneur en composés .....................................................................................18

10.2.1 Quantification par rapport au FRSC .............................................................................................................18

10.2.2 Quantification par rapport à l’étalon de substitution ...................................................................18

11 Calcul de la teneur en COV et en COSV .........................................................................................................................................18

11.1 Généralités ...............................................................................................................................................................................................18

11.2 Méthode 1 — Teneur en COV et/ou en COSV, en pourcentage en masse, du produit

« prêt à l’emploi »...............................................................................................................................................................................19

11.3 Méthode 2 — Teneur en COV et/ou en COSV, en grammes par litre, du produit

« prêt à l’emploi »...............................................................................................................................................................................19

11.4 Méthode 3 — Teneur en COV et/ou en COSV, en grammes par litre, du produit

« prêt à l’emploi » moins l’eau ................................................................................................................................................20

11.5 Méthode 4 — Teneur en COV et/ou en COSV, en grammes par litre, du produit

« prêt à l’emploi » moins l’eau et moins les composés exempts ...............................................................20

12 Évaluation des données et calcul du résultat final .........................................................................................................21

13 Fidélité .........................................................................................................................................................................................................................22

13.1 Généralités ...............................................................................................................................................................................................22

13.2 Limite de répétabilité, r ................................................................................................................................................................ 22

13.3 Limite de reproductibilité, R .................................................................................................................................................... 22

14 Rapport d’essai ....................................................................................................................................................................................................22

Annexe A (normative) Liste non exhaustive des composés COV, COSV et CONV ...................................................24

© ISO 2020 – Tous droits réservés iii
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ISO 11890-2:2020(F)

Annexe B (informative) Informations sur les produits thermiquement instables ...........................................30

Annexe C (informative) Exemples de conditions pour la méthode CG ...........................................................................37

Annexe D (informative) Résultats de l’essai interlaboratoires pour la détermination des

données de fidélité ..........................................................................................................................................................................................39

Bibliographie ...........................................................................................................................................................................................................................41

iv © ISO 2020 – Tous droits réservés
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ISO 11890-2:2020(F)
Avant-propos

L’ISO (Organisation internationale de normalisation) est une fédération mondiale d’organismes

nationaux de normalisation (comités membres de l’ISO). L’élaboration des Normes internationales est

en général confiée aux comités techniques de l’ISO. Chaque comité membre intéressé par une étude

a le droit de faire partie du comité technique créé à cet effet. Les organisations internationales,

gouvernementales et non gouvernementales, en liaison avec l’ISO participent également aux travaux.

L’ISO collabore étroitement avec la Commission électrotechnique internationale (IEC) en ce qui

concerne la normalisation électrotechnique.

Les procédures utilisées pour élaborer le présent document et celles destinées à sa mise à jour sont

décrites dans les Directives ISO/IEC, Partie 1. Il convient, en particulier, de prendre note des différents

critères d’approbation requis pour les différents types de documents ISO. Le présent document a été

rédigé conformément aux règles de rédaction données dans les Directives ISO/IEC, Partie 2 (voir www

.iso .org/ directives).

L’attention est attirée sur le fait que certains des éléments du présent document peuvent faire l’objet de

droits de propriété intellectuelle ou de droits analogues. L’ISO ne saurait être tenue pour responsable

de ne pas avoir identifié de tels droits de propriété et averti de leur existence. Les détails concernant

les références aux droits de propriété intellectuelle ou autres droits analogues identifiés lors de

l’élaboration du document sont indiqués dans l’Introduction et/ou dans la liste des déclarations de

brevets reçues par l’ISO (voir www .iso .org/ brevets).

Les appellations commerciales éventuellement mentionnées dans le présent document sont données

pour information, par souci de commodité, à l’intention des utilisateurs et ne sauraient constituer un

engagement.

Pour une explication de la nature volontaire des normes, la signification des termes et expressions

spécifiques de l’ISO liés à l’évaluation de la conformité, ou pour toute information au sujet de l’adhésion

de l’ISO aux principes de l’Organisation mondiale du commerce (OMC) concernant les obstacles

techniques au commerce (OTC), voir le lien suivant: www .iso .org/ iso/ fr/ avant -propos .html.

Le présent document a été élaboré par le comité technique ISO/TC 35, Peintures et vernis, en collaboration

avec le comité technique CEN/TC 139, Peintures et vernis, du Comité européen de normalisation (CEN),

conformément à l’Accord de coopération technique entre l’ISO et le CEN (Accord de Vienne).

Cette quatrième édition annule et remplace la troisième édition (ISO 11890-2:2013), dont elle constitue

une révision technique.

Les principales modifications par rapport à l’édition précédente sont les suivantes:

— le domaine d’application a été élargi pour inclure la détermination des composés organiques semi-

volatils (COSV);

— le domaine d’application a été élargi pour inclure les plages de concentration allant de 0,01 % à 100 %;

— les spécifications concernant la détermination des composés organiques semi-volatils ont été

ajoutées.

Une liste de toutes les parties de la série ISO 11890 se trouve sur le site web de l’ISO.

Il convient que l’utilisateur adresse tout retour d’information ou toute question concernant le présent

document à l’organisme national de normalisation de son pays. Une liste exhaustive desdits organismes

se trouve à l’adresse www .iso .org/ fr/ members .html.
© ISO 2020 – Tous droits réservés v
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ISO 11890-2:2020(F)
Introduction

Le présent document fait partie d’une série de normes qui traitent de l’échantillonnage et des essais

relatifs aux produits de peinture et à leurs matières premières. Il spécifie une méthode pour la

détermination de la teneur en composés organiques volatils (COV) et en composés organiques semi-

volatils (COSV) des produits de peinture et de leurs matières premières.
vi © ISO 2020 – Tous droits réservés
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NORME INTERNATIONALE ISO 11890-2:2020(F)
Peintures et vernis — Détermination de la teneur en
composés organiques volatils (COV) et/ou composés
organiques semi-volatils (COSV) —
Partie 2:
Méthode par chromatographie en phase gazeuse

AVERTISSEMENT — Le présent document peut impliquer l’utilisation de produits et la mise en

œuvre de modes opératoires et d’appareillages à caractère dangereux. Le présent document

n’a pas pour but d’aborder tous les problèmes de sécurité liés à son utilisation. Il incombe aux

utilisateurs du présent document de prendre des mesures appropriées pour assurer la santé

et la sécurité du personnel avant l’application du document, et de déterminer l’applicabilité de

toute autre restriction éventuelle.
1 Domaine d’application

Le présent document est applicable à la détermination des COV et des COSV pour lesquels la teneur

attendue en COV et/ou en COSV est supérieure à 0,01 % en masse et jusqu’à 100 % en masse.

La méthode donnée dans l’ISO 11890-1 est utilisée lorsque la teneur en COV est supérieure à 15 % en

masse. Le présent document (méthode ISO 11890-2) s’applique lorsque le système contient des COV et

des COSV, car le résultat obtenu selon l’ISO 11890-1 peut être influencé par les COSV. Pour une teneur

en COV inférieure à 0,1 %, la méthode de l’espace de tête décrite dans l’ISO 17895 est utilisée en guise

d’alternative. L’ISO 11890-1 et l’ISO 17895 ne peuvent pas être utilisées pour la détermination de la

teneur en COSV.

NOTE 1 Certains ingrédients des produits de peinture et de leurs matières premières peuvent se décomposer

pendant l’analyse et causer des signaux COV et/ou COSV artificiels. Lors de la détermination des COV et/ou des

COSV dans les produits de peinture et leurs matières premières, ces signaux sont des artefacts de la méthode et

ne sont pas pris en compte (des exemples sont donnés à l’Annexe B).

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 adaptée et d’en tenir compte dans les calculs. La méthode définie dans le présent

document n’est pas applicable à la détermination de la teneur en eau.

NOTE 2 Si des acides ou des bases organiques et leurs sels correspondants sont présents dans le produit de

peinture ou ses matières premières, la quantité qui est quantifiée par cette méthode pourrait ne pas être exacte

en raison d’une modification de l’équilibre acido-basique.
2 Références normatives

Les documents suivants sont cités dans le texte de sorte qu’ils constituent, pour tout ou partie de leur

contenu, des exigences du présent document. Pour les références datées, seule l’édition citée s’applique.

Pour les références non datées, la dernière édition du document de référence s’applique (y compris les

éventuels amendements).
ISO 760, Dosage de l'eau — Méthode de Karl Fischer (Méthode générale)

ISO 1513, Peintures et vernis — Examen et préparation des échantillons pour essai

ISO 2811 (toutes les parties), Peintures et vernis — Détermination de la masse volumique

ISO 15528, Peintures, vernis et matières premières pour peintures et vernis — Échantillonnage

© ISO 2020 – Tous droits réservés 1
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ISO 11890-2:2020(F)
3 Termes et définitions

Pour les besoins du présent document, les termes et définitions suivants s’appliquent.

L’ISO et l’IEC tiennent à jour des bases de données terminologiques destinées à être utilisées en

normalisation, consultables aux adresses suivantes:

— ISO Online browsing platform: disponible à l’adresse https:// www .iso .org/ obp;

— IEC Electropedia: disponible à l’adresse http:// www .electropedia .org/ .
3.1
composé organique volatil
COV

tout liquide et/ou solide organique qui s’évapore spontanément à la température et à la pression de

l’atmosphère avec laquelle il est en contact

Note 1 à l'article: Concernant l’usage du terme COV dans le domaine des produits de peinture, voir teneur en

composés organiques volatils (teneur en COV) (3.4).

Note 2 à l'article: Dans certaines réglementations aux États-Unis, le terme COV est uniquement utilisé pour les

composés qui ont une activité photochimique dans l’atmosphère (voir l’ASTM D3960). Tous les autres composés

sont alors définis comme des composés exempts (3.6).
[SOURCE: ISO 4618:2014, 2.270]
3.2
composé organique semi-volatil
COSV

liquide et/ou solide organique qui s’évapore spontanément, mais plus lentement qu’un COV à la

température et à la pression de l’atmosphère avec laquelle il est en contact

Note 1 à l'article: Concernant l’usage du terme COSV dans le domaine des produits de peinture, voir teneur en

composés organiques semi-volatils (teneur en COSV) (3.5).
3.3
composé organique non volatil
CONV

liquide et/ou solide organique qui n’est pas classifié comme étant un COV ou un COSV

3.4
teneur en composés organiques volatils
teneur en COV
TCOV

masse des composés organiques volatils (3.1) présents dans un produit de peinture, déterminée dans des

conditions spécifiées

Note 1 à l'article: Les propriétés et la quantité des composés à prendre en compte dépendent du domaine

d’application du produit de peinture. Pour chaque domaine d’application, les valeurs limites et les méthodes de

détermination ou de calcul sont stipulées par des réglementations ou par des accords.

Note 2 à l'article: Si le terme COV désigne des composés ayant un point d’ébullition maximal défini, les composés

considérés comme entrant dans la teneur en COV sont ceux ayant un point d’ébullition inférieur à cette limite

incluse, les composés ayant un point d’ébullition supérieur étant considérés comme des composés organiques

semi-volatils ou non volatils.
[SOURCE: ISO 4618:2014, 2.271 modifiée — Note 2 à l’article ajoutée]
2 © ISO 2020 – Tous droits réservés
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ISO 11890-2:2020(F)
3.5
teneur en composés organiques semi-volatils
teneur en COSV
TCOSV

masse des composés organiques semi-volatils (3.2) présents dans un produit de peinture, déterminée

dans des conditions spécifiées

Note 1 à l'article: Les propriétés et la quantité des composés à prendre en compte dépendent du domaine

d’application du produit de peinture. Pour chaque domaine d’application, les valeurs limites et les méthodes de

détermination ou de calcul sont stipulées par des réglementations ou par des accords.

Note 2 à l'article: Si le terme COSV désigne des composés ayant un point d’ébullition maximal et un point

d’ébullition minimal définis, les composés considérés comme entrant dans la teneur en COSV sont ceux ayant

un point d’ébullition inférieur à cette limite supérieure incluse et supérieur à cette limite inférieure incluse, les

composés ayant un point d’ébullition supérieur étant considérés comme des composés organiques non volatils.

3.6
composé exempt

composé organique qui ne participe pas à des réactions photochimiques dans l’atmosphère

Note 1 à l'article: Cette expression n’est pas pertinente dans certains pays.
3.7
prêt à l’emploi

état d’un produit, une fois mélangé conformément aux instructions du fabricant, dans les bonnes

proportions et dilué, si nécessaire, à l’aide de diluants appropriés, de sorte que la peinture puisse être

appliquée selon la méthode approuvée
3.8
étalon interne

composé qui n’est pas présent dans l’échantillon et qui est complètement séparé des autres éléments du

chromatogramme, qui est inerte par rapport aux constituants de l’échantillon, stable dans la plage de

températures requise et de pureté connue et qui est ajouté à l’échantillon pour contrôler la dilution et

l’étape d’injection de l’analyse
3.9
étalon de substitution

composé de pureté connue qui est utilisé pour quantifier les COV et COSV non identifiés

3.10
composé marqueur

composé servant à différencier les COV des COSV, ou les COSV des CONV, si la différenciation doit être

réalisée sur la base du temps de rétention (3.11)
3.11
temps de rétention

temps écoulé entre l’injection du composant échantillon et l’enregistrement du pic maximal

3.12
solvant d’extraction
liquide utilisé pour extraire les COV et les COSV de la matrice étudiée
3.13
pic principal
pic qui contribue de manière significative:

— à la teneur en COV, c’est-à-dire ≥ 10 % de la teneur en COV absolue (en équivalents DEA) et ≥ 0,1 %

en masse (en équivalents DEA); ou

— à la teneur en COSV, c’est-à-dire ≥ 10 % de la teneur en COSV absolue (en équivalents DEA) et ≥ 0,1 %

en masse (en équivalents DEA)
© ISO 2020 – Tous droits réservés 3
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ISO 11890-2:2020(F)
3.14
pic secondaire
pic qui contribue seulement dans une faible mesure:

— à la teneur en COV, c’est-à-dire < 0,1 % en masse (en équivalents DEA) et/ou < 10 % de la teneur en

COV absolue (en équivalents DEA); ou

— à la teneur en COSV, c’est-à-dire < 0,1 % en masse (en équivalents DEA) et/ou < 10 % de la teneur en

COSV absolue (en équivalents DEA)
3.15
réactif
substance utilisée dans une analyse chimique/biochimique ou d’autres réactions
[SOURCE: ISO 20391-1:2018, 3.19]
4 Principe

Une fois l’échantillon préparé, les COV, COSV et CONV sont séparés par chromatographie en phase

gazeuse. Selon le type d’échantillon, on utilise un système d’injection de l’échantillon à chaud ou à froid.

La méthode préconisée est l’injection à chaud. Une fois identifiés, par exemple par CG-SM, les composés

sont quantifiés à partir des aires de pics par rapport à la réponse relative spécifique de leur composé, au

moyen d’un étalon interne par CG-DIF. Les substances non identifiables sont quantifiées par rapport à

un étalon de substitution pouvant être identique à l’étalon interne. Un calcul permet d’obtenir la teneur

en COV et/ou en COSV de l’échantillon.
5 Informations requises

Pour toute application particulière, il convient que les informations requises fassent, de préférence,

l’objet d’un accord entre les parties intéressées, ces informations pouvant être issues, en totalité ou en

partie, d’une Norme internationale ou nationale ou de tout autre document relatif au produit soumis à

l’essai.
Les informations requises peuvent inclure les éléments suivants:
a) le(s) composé(s) organique(s) à déterminer (voir l’Article 9);
b) les conditions expérimentales à appliquer (voir 8.5);
c) les critères de classification en COV et/ou COSV;

d) l’indication des composés organiques mentionnés en a) qui sont des composés exempts (le cas

échéant);
e) la méthode de calcul à utiliser (voir l’Article 10 et l’Article 11).
6 Appareillage
6.1 Chromatographe en phase gazeuse

Toutes les parties de l’instrument en contact avec l’échantillon pour essai doivent être constituées d’un

matériau (par exemple du verre) qui résiste à l’échantillon et qui n’est pas susceptible de le modifier

chimiquement.
Utiliser l’un des deux types spécifiés en 6.1.1 et 6.1.2.
4 © ISO 2020 – Tous droits réservés
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ISO 11890-2:2020(F)
6.1.1 Système d’injection à chaud (système recommandé)

L’instrument doit comporter un bloc d’injection à température variable avec un diviseur d’échantillon.

La température d’injection doit être réglable, avec une précision de 1 °C. La température d’utilisation

normale doit être comprise entre 250 °C et 280 °C.

NOTE Il est judicieux d’utiliser de la laine de verre silanée pour retenir les constituants non volatils. Les

côtés actifs de la laine de verre silanée peuvent être un puits pour les composés organiques et influencer de

manière significative le taux de récupération dans la plage inférieure de la méthode. L’adsorption se manifeste

par une traînée du pic, surtout dans le cas des composants peu volatils et/ou de polarité élevée.

6.1.2 Système d’injection à froid (vaporisateur à température programmée, VTP)

Le système d’injection à froid doit être muni d’un dispositif de programmation de la température,

incluant un diviseur d’échantillon pour l’opération de division, permettant de passer de la température

ambiante à 300 °C.

NOTE Il est judicieux d’utiliser de la laine de verre silanée pour retenir les constituants non volatils. Les

côtés actifs de la laine de verre silanée peuvent être un puits pour les composés organiques et influencer de

manière significative le taux de récupération dans la plage inférieure de la méthode. L’adsorption se manifeste

par une traînée du pic, surtout dans le cas des composants peu volatils et/ou de polarité élevée.

6.1.3 Choix du système d’injection de l’échantillon

Le choix d’un système d’injection à chaud ou à froid dépend du type de produit soumis à l’essai. Il est

préférable d’utiliser le système d’injection à froid pour les produits qui, à haute température, dégagent

des substances qui influent sur la détermination. Les produits de clivage des liants ou des additifs

peuvent être réduits par l’utilisation d’un système d’injection à froid.

Des changements intervenant dans le chromatogramme (par exemple la présence de pics étrangers

ou une augmentation ou diminution de la taille des pics) indiquent des réactions de clivage ou de

décomposition selon les températures d’injection de l’échantillon (voir l’Annexe B).

6.2 Étuve

L’étuve doit pouvoir être chauffée entre 40 °C et 300 °C, tant en isotherme qu’en programmation de

température. Il doit être possible de régler la température de l’étuve à 1 °C près. La température finale

du programme de température ne doit pas dépasser la température maximale d’utilisation de la colonne

capillaire (voir 6.4).
6.3 Détecteur
Les deux détecteurs suivants doivent être utilisés.

6.3.1 Spectromètre de masse ou autre détecteur sélectif de masse (SM ou DSM), pour

l’identification des composés COV et COSV. Pour éviter les risques de condensation, la température du

détecteur doit être supérieure d’au moins 10 °C à la température maximale de l’étuve.

6.3.2 Détecteur à ionisation de flamme (DIF), pour la quantification des composés COV et

COSV, fonctionnant à des températures comprises entre 230 °C et 300 °C. Pour éviter les risques de

condensation, la température du détecteur doit être supérieure d’au moins 10 °C à la température

maximale de l’étuve. L’alimentation en gaz du détecteur, le volume d’injection, le rapport de division et

le réglage du gain doivent être optimisés de sorte que les signaux (aire des pics) utilisés pour le calcul

soient proportionnels à la quantité de substance.
6.4 Colonne capillaire

La colonne doit être constituée de verre ou de silice fondue. Des colonnes ayant une longueur suffisante

pour séparer les composés volatils et un diamètre intérieur maximal de 0,32 mm, revêtues de 5 % de

© ISO 2020 – Tous droits réservés 5
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ISO 11890-2:2020(F)

poly(diméthylsiloxane) phényle modifié ou de 6 % de (cyanopropylphényl)-méthylpolysiloxane avec

une épaisseur de film appropriée, doivent être utilisées.
...