Paints and varnishes -- Determination of solvents in coating materials containing organic solvents only -- Gas-chromatographic method

This document specifies a method for the gas-chromatographic determination of the qualitative and quantitative composition of solvents contained in a product. The method is applicable to coating materials containing solely organic solvents (generally called conventional coating materials) and binder solutions and non-aqueous dispersions containing solely organic solvents. The method defined in this document is not applicable for determination of volatile organic compounds (VOC) and semi-volatile organic compounds (SVOC) content. NOTE For determination of VOC and SVOC, see ISO 11890-2.

Peintures et vernis -- Détermination des solvants dans les produits de peinture contenant uniquement des solvants organiques -- Méthode par chromatographie en phase gazeuse

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Published
Publication Date
18-Mar-2021
Current Stage
5060 - Close of voting Proof returned by Secretariat
Start Date
24-Dec-2020
Completion Date
23-Dec-2020
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INTERNATIONAL ISO
STANDARD 23322
First edition
2021-03
Paints and varnishes — Determination
of solvents in coating materials
containing organic solvents only —
Gas-chromatographic method
Peintures et vernis — Détermination des solvants dans les produits de
peinture contenant uniquement des solvants organiques — Méthode
par chromatographie en phase gazeuse
Reference number
ISO 23322:2021(E)
ISO 2021
---------------------- Page: 1 ----------------------
ISO 23322:2021(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2021

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: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2021 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 23322:2021(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

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

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

3 Terms and definitions ..................................................................................................................................................................................... 1

4 Units ................................................................................................................................................................................................................................... 1

5 Principle ........................................................................................................................................................................................................................ 1

6 Apparatus ..................................................................................................................................................................................................................... 2

6.1 Gas chromatograph ............................................................................................................................................................................. 2

6.1.1 General...................................................................................................................................................................................... 2

6.1.2 Sample injection system ............................................................................................................................................ 2

6.1.3 Oven ............................................................................................................................................................................................ 2

6.1.4 Detector ................................................................................................................................................................................... 3

6.1.5 Capillary separation column .................................................................................................................................. 3

6.1.6 Analytical system performance criteria ....................................................................................................... 3

6.2 Injection syringe .................................................................................................................................................................................... 3

6.3 Data processing ...................................................................................................................................................................................... 3

6.4 Sample vial ................................................................................................................................................................................................ 3

7 Reagents ........................................................................................................................................................................................................................ 4

7.1 General .......................................................................................................................................................................................................... 4

7.2 Internal standard .................................................................................................................................................................................. 4

7.3 Gases ................................................................................................................................................................................................................ 4

7.4 Calibration substances ..................................................................................................................................................................... 4

7.5 Extraction solvent ................................................................................................................................................................................. 4

8 Sampling ........................................................................................................................................................................................................................ 5

9 Choice of sample injection system ..................................................................................................................................................... 5

10 Procedure..................................................................................................................................................................................................................... 5

10.1 Gas chromatographic conditions ............................................................................................................................................. 5

10.2 Injection volume .................................................................................................................................................................................... 5

10.3 Calibration .................................................................................................................................................................................................. 5

10.3.1 General...................................................................................................................................................................................... 5

10.3.2 Preparation of calibration solutions ............................................................................................................... 5

10.3.3 Analysis of the multi-point calibration ......................................................................................................... 6

10.4 Quality assurance.................................................................................................................................................................................. 7

10.5 Sample preparation and analysis ............................................................................................................................................ 7

10.5.1 Direct injection .................................................................................................................................................................. 7

10.5.2 Head space injection ..................................................................................................................................................... 7

10.5.3 Preparation of test samples for analysis without multiple standard additions ........ 7

10.5.4 Data acquisition for sample measurement ............................................................................................... 8

11 Quantitative determination of compound content with respect to CSRF ..................................................8

12 Expression of results ........................................................................................................................................................................................ 8

13 Precision ....................................................................................................................................................................................................................... 8

13.1 Repeatability ............................................................................................................................................................................................. 8

13.2 Reproducibility ....................................................................................................................................................................................... 9

14 Test report ................................................................................................................................................................................................................... 9

Annex A (informative) Examples for GC method conditions ....................................................................................................10

Bibliography .............................................................................................................................................................................................................................13

© ISO 2021 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 23322:2021(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, Subcommittee

SC 16, Chemical analysis.

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.
iv © ISO 2021 – All rights reserved
---------------------- Page: 4 ----------------------
INTERNATIONAL STANDARD ISO 23322:2021(E)
Paints and varnishes — Determination of solvents in
coating materials containing organic solvents only — Gas-
chromatographic method
1 Scope

This document specifies a method for the gas-chromatographic determination of the qualitative and

quantitative composition of solvents contained in a product. The method is applicable to coating

materials containing solely organic solvents (generally called conventional coating materials) and

binder solutions and non-aqueous dispersions containing solely organic solvents.

The method defined in this document is not applicable for determination of volatile organic compounds

(VOC) and semi-volatile organic compounds (SVOC) content.
NOTE For determination of VOC and SVOC, see ISO 11890-2.
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 4618, Paints and varnishes — Terms and definitions

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

3 Terms and definitions

For the purposes of this document, the terms and definitions given in ISO 4618 apply.

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

— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org/
4 Units
The analytical results are expressed as a mass fraction.
5 Principle

The volatile fraction of the sample of product under test is separated by gas chromatography. Either

a hot sample injection system, a cold sample injection system or a headspace injection system can be

used, depending on the product type. After the components have been identified, they are quantified

from the peak areas using the internal standard method.
© ISO 2021 – All rights reserved 1
---------------------- Page: 5 ----------------------
ISO 23322:2021(E)
6 Apparatus
6.1 Gas chromatograph
6.1.1 General

The gas chromatograph shall be suitable for use with capillary separation columns and meet the

conditions specified in 6.1.2 to 6.1.4.

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.
6.1.2 Sample injection system
6.1.2.1 General
The method provides a choice between three sample injection systems:
— hot-injection system with sample splitter;
— cold-injection system with sample splitter;
— headspace injector.
6.1.2.2 Hot-injection 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 K. 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.
6.1.2.3 Cold-injection system

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.
6.1.2.4 Headspace injection
It shall be possible to set the following values:
— controlled sample temperature: 150 °C;
— controlled transfer line and dispensing valve temperatures: 160 °C;
— temperature hold time: 4 min.
6.1.3 Oven

The oven shall be capable of being heated between 40 °C and 300 °C, both isothermally and under

programmed temperature control. It shall be possible to set the oven temperature to within 1 K. The

2 © ISO 2021 – All rights reserved
---------------------- Page: 6 ----------------------
ISO 23322:2021(E)

final temperature of the temperature program shall not exceed the maximum operating temperature of

the separation column (see manufacturer's instructions).
6.1.4 Detector
6.1.4.1 General
One of the following two detectors shall be used.
6.1.4.2 Mass spectrometer (MS) or other mass-selective detector (MSD)

To prevent condensation, the detector temperature shall be at least 10 K above the maximum oven

temperature.
6.1.4.3 Flame ionization detector

The flame ionization detector (FID) is operated at temperatures between 230 °C and 300 °C. To prevent

condensation, the detector temperature shall be at least 10 K above the maximum oven temperature.

The detector gas supply, injection volume, split ratio and gain setting shall be optimized so that the

signals (peak areas) used for the calculation are proportional to the amount of substance.

6.1.5 Capillary separation column
The column shall be made of glass or fused silica. Column
...

FINAL
INTERNATIONAL ISO/FDIS
DRAFT
STANDARD 23322
ISO/TC 35
Paints and varnishes — Determination
Secretariat: NEN
of solvents in coating materials
Voting begins on:
2020­10­28 containing organic solvents only —
Gas-chromatographic method
Voting terminates on:
2020­12­23
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 23322:2020(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 23322:2020(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
CH­1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2020 – All rights reserved
---------------------- Page: 2 ----------------------
ISO/FDIS 23322:2020(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

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

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

3 Terms and definitions ..................................................................................................................................................................................... 1

4 Units ................................................................................................................................................................................................................................... 1

5 Principle ........................................................................................................................................................................................................................ 1

6 Apparatus ..................................................................................................................................................................................................................... 2

6.1 Gas chromatograph ............................................................................................................................................................................. 2

6.1.1 General...................................................................................................................................................................................... 2

6.1.2 Sample injection system ............................................................................................................................................ 2

6.1.3 Oven ............................................................................................................................................................................................ 2

6.1.4 Detector ................................................................................................................................................................................... 3

6.1.5 Capillary separation column .................................................................................................................................. 3

6.1.6 Analytical system performance criteria ....................................................................................................... 3

6.2 Injection syringe .................................................................................................................................................................................... 3

6.3 Data processing ...................................................................................................................................................................................... 3

6.4 Sample vial ................................................................................................................................................................................................ 3

7 Reagents ........................................................................................................................................................................................................................ 4

7.1 General .......................................................................................................................................................................................................... 4

7.2 Internal standard .................................................................................................................................................................................. 4

7.3 Gases ................................................................................................................................................................................................................ 4

7.4 Calibration substances ..................................................................................................................................................................... 4

7.5 Extraction solvent ................................................................................................................................................................................. 4

8 Sampling ........................................................................................................................................................................................................................ 5

9 Choice of sample injection system ..................................................................................................................................................... 5

10 Procedure..................................................................................................................................................................................................................... 5

10.1 Gas chromatographic conditions ............................................................................................................................................. 5

10.2 Injection volume .................................................................................................................................................................................... 5

10.3 Calibration .................................................................................................................................................................................................. 5

10.3.1 General...................................................................................................................................................................................... 5

10.3.2 Preparation of calibration solutions ............................................................................................................... 5

10.3.3 Analysis of the multi-point calibration ......................................................................................................... 6

10.4 Quality assurance.................................................................................................................................................................................. 7

10.5 Sample preparation and analysis ............................................................................................................................................ 7

10.5.1 Direct injection .................................................................................................................................................................. 7

10.5.2 Head space injection ..................................................................................................................................................... 7

10.5.3 Preparation of test samples for analysis without multiple standard additions ........ 7

10.5.4 Data acquisition for sample measurement ............................................................................................... 7

11 Quantitative determination of compound content with respect to CSRF ..................................................8

12 Expression of results ........................................................................................................................................................................................ 8

13 Precision ....................................................................................................................................................................................................................... 8

13.1 Repeatability ............................................................................................................................................................................................. 8

13.2 Reproducibility ....................................................................................................................................................................................... 9

14 Test report ................................................................................................................................................................................................................... 9

Annex A (informative) Examples for GC method conditions ....................................................................................................10

Bibliography .............................................................................................................................................................................................................................13

© ISO 2020 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO/FDIS 23322:2020(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 non­governmental, 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.

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.
iv © ISO 2020 – All rights reserved
---------------------- Page: 4 ----------------------
FINAL DRAFT INTERNATIONAL STANDARD ISO/FDIS 23322:2020(E)
Paints and varnishes — Determination of solvents in
coating materials containing organic solvents only — Gas-
chromatographic method
1 Scope

This document specifies a method for the gas-chromatographic determination of the qualitative and

quantitative composition of solvents contained in a product. The method is applicable to coating

materials containing solely organic solvents (generally called conventional coating materials) and

binder solutions and non-aqueous dispersions containing solely organic solvents.

The method defined in this document is not applicable for determination of volatile organic compounds

(VOC) and semi­volatile organic compounds (SVOC) content.
NOTE For determination of VOC and SVOC, see ISO 11890­2.
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 4618, Paints and varnishes — Terms and definitions

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

3 Terms and definitions

For the purposes of this document, the terms and definitions given in ISO 4618 apply.

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

— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org/
4 Units
The analytical results are expressed as a mass fraction.
5 Principle

The volatile fraction of the sample of product under test is separated by gas chromatography. Either

a hot sample injection system, a cold sample injection system or a headspace injection system can be

used, depending on the product type. After the components have been identified, they are quantified

from the peak areas using the internal standard method.
© ISO 2020 – All rights reserved 1
---------------------- Page: 5 ----------------------
ISO/FDIS 23322:2020(E)
6 Apparatus
6.1 Gas chromatograph
6.1.1 General

The gas chromatograph shall be suitable for use with capillary separation columns and meet the

conditions specified in 6.1.2 to 6.1.4.

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.
6.1.2 Sample injection system
6.1.2.1 General
The method provides a choice between three sample injection systems:
— hot-injection system with sample splitter;
— cold-injection system with sample splitter;
— headspace injector.
6.1.2.2 Hot-injection system

The instrument shall have a variable­temperature injection block with sample splitter. The injection

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

be between 250 °C and 280 °C.

NOTE It is useful to use silanized glass wool to retain non­volatile 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.
6.1.2.3 Cold-injection system

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 non­volatile 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.
6.1.2.4 Headspace injection
It shall be possible to set the following values:
— controlled sample temperature: 150 °C;
— controlled transfer line and dispensing valve temperatures: 160 °C;
— temperature hold time: 4 min.
6.1.3 Oven

The oven shall be capable of being heated between 40 °C and 300 °C, both isothermally and under

programmed temperature control. It shall be possible to set the oven temperature to within 1 K. The

2 © ISO 2020 – All rights reserved
---------------------- Page: 6 ----------------------
ISO/FDIS 23322:2020(E)

final temperature of the temperature program shall not exceed the maximum operating temperature of

the separation column (see manufacturer's instructions).
6.1.4 Detector
6.1.4.1 General
One of the following two detectors shall be used.
6.1.4.2 Mass spectrometer (MS) or other mass-selective detector (MSD)

To prevent condensation, the detector temperature shall be at least 10 K above the maximum oven

temperature.
6.1.4.3 Flame ionization detector

The flame ionization detector (FID) is operated at temperatures between 230 °C and 300 °C. To prevent

condensation, the detector temperature shall be at least 10 K above the maximum oven temperature.

The detector gas supply, injection volume, split ratio and gain setting s
...

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