ISO 16000-33:2024
(Main)Indoor air — Part 33: Determination of phthalates with gas chromatography/mass spectrometry (GC/MS)
Indoor air — Part 33: Determination of phthalates with gas chromatography/mass spectrometry (GC/MS)
This document specifies the sampling and analysis of phthalates in indoor air and describes the sampling and analysis of phthalates in house dust and in solvent wipe samples of surfaces by means of gas chromatography-mass spectrometry (GC-MS). Two alternative sampling, sample preparation and sample introduction methods, whose comparability has been proven in an interlaboratory test, are specified for indoor air[1]: — sorbent tubes sampling with subsequent thermal desorption GC-MS, and — sampling by adsorption and subsequent solvent extraction and injection to GC-MS. Additional adsorbents that can be used are described in Annex B. Depending on the sampling method, the compounds dimethyl phthalate to diisoundecylphthalate can be analysed in house dust as described in Annex D. The investigation of house dust samples is only appropriate as a screening method. This investigation only results in indicative values and is not acceptable for a final assessment of a potential need for action. Dimethyl phthalate to diisoundecylphthalate can be analysed in solvent wipe samples as described in Annex C. Solvent wipe samples are suitable for non-quantitative source identification. NOTE In principle, the method is also suitable for the analysis of other phthalates, adipates and cyclohexane dicarboxylic acid esters, but this is confirmed by determination of the performance characteristics in each case. General information on phthalates are given in Annex A.
Air intérieur — Partie 33: Détermination des phthalates par chromatographie en phase gazeuse/spectrométrie de masse (CPG/SM)
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International
Standard
ISO 16000-33
Second edition
Indoor air —
2024-07
Part 33:
Determination of phthalates
with gas chromatography/mass
spectrometry (GC/MS)
Air intérieur —
Partie 33: Détermination des phthalates par chromatographie en
phase gazeuse/spectrométrie de masse (CPG/SM)
Reference number
© ISO 2024
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
Contents Page
Foreword .v
Introduction .vi
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Abbreviated terms . 2
5 Sampling methods and analytical apparatus. 3
5.1 General .3
5.2 Sampling by adsorption with subsequent thermal desorption .3
5.2.1 Apparatus, operating materials and chemicals .3
5.2.2 Preparation of the thermal desorption tube .4
5.2.3 Sampling .4
5.3 Sampling by adsorption and subsequent solvent extraction .5
5.3.1 Apparatus, operating materials and chemicals .5 ®
5.3.2 Preparation of Florisil and the adsorption tubes .6 ®
5.3.3 Suggestions regarding the application of Florisil .6
5.3.4 Sampling .7
5.3.5 Sample conditioning .7
6 Calibration . 8
6.1 General .8
6.2 Calibration of the thermal desorption method .8
6.3 Calibration of the solvent extraction method .8
7 Identification and quantification . 9
7.1 Mass spectrometric analysis .9
8 Establishment of calibration curves and calculation of the analyte mass. 14
8.1 Establishment of a calibration curve .14
8.2 Calculation of the analyte mass . .14
9 Calculation of indoor air concentrations .15
10 Performance characteristics . 16
10.1 Detection limit .16
10.2 Quantification limit and problems related to blank values .16
10.3 Reproducibility standard deviation and repeatability standard deviation .17
11 Quality assurance .18
11.1 Method verification and determination of blanks .18
11.1.1 General .18
11.1.2 Field blank value of the indoor air .18
11.1.3 Analytical laboratory blank value .18
11.2 Measures for blank value minimization .18
11.3 Documents.19
12 Interferences . 19
Annex A (informative) General information on phthalates .20
Annex B (informative) Sampling by adsorption with ODS solid phase disk or SDB copolymer
cartridge .23
Annex C (informative) Screening phthalates in solvent wipe tests .29
Annex D (informative) Screening phthalates in house dust .32
Annex E (informative) Practical example for the calibration of the thermal desorption method .36
iii
Annex F (informative) Practical example for the calibration of the solvent extraction method ®
using Florisil .38
Annex G (informative) Practical example for the gas chromatography with thermal desorption .40
Annex H (informative) Practical example for the gas chromatography following solvent
extraction . 41
Annex I (informative) Problems related to the blank values .42
Annex J (informative) Example of sampling protocol documentation .43
Bibliography .44
iv
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 document 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).
ISO draws attention to the possibility that the implementation of this document may involve the use of (a)
patent(s). ISO takes no position concerning the evidence, validity or applicability of any claimed patent
rights in respect thereof. As of the date of publication of this document, ISO had not received notice of (a)
patent(s) which may be required to implement this document. However, implementers are cautioned that
this may not represent the latest information, which may be obtained from the patent database available at
www.iso.org/patents. ISO shall not be held responsible for identifying any or all such patent rights.
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 146, Air quality, Subcommittee SC 6, Indoor air.
This second edition cancels and replaces the first edition (ISO 16000-33:2017), which has been technically
revised.
The main change is as follows: a description of an adsorbent which can alternatively be used has been added.
A list of all parts in the ISO 16000 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.
v
Introduction
Different parts of the ISO 16000 series describe the general requirements relating to the measurement of
indoor air pollutants and the important conditions to be observed before or during the sampling of individual
pollutants or groups of pollutants, as well as the measurement procedures themselves.
The definition of indoor environment is given by ISO 16000-1. Dwellings [living rooms, bedrooms, do-it-
yourself (DIY) rooms, sports rooms and cellars, kitchens and bathrooms], workrooms or workplaces in
buildings which are not subject to health and safety inspections with respect to air pollutants (e.g. offices,
salesrooms), public buildings (e.g. restaurants, theatres, cinemas and other meeting rooms) and passenger
cabins of motor vehicles and public transport are among the
...
FINAL DRAFT
International
Standard
ISO/FDIS 16000-33
ISO/TC 146/SC 6
Indoor air —
Secretariat: DIN
Part 33:
Voting begins on:
2024-03-08
Determination of phthalates
with gas chromatography/mass
Voting terminates on:
2024-05-03
spectrometry (GC/MS)
RECIPIENTS OF THIS DRAFT ARE INVITED TO SUBMIT,
WITH THEIR COMMENTS, NOTIFICATION OF ANY
RELEVANT PATENT RIGHTS OF WHICH THEY ARE AWARE
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BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO-
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.
Reference number
ISO/FDIS 16000-33:2024(en) © ISO 2024
FINAL DRAFT
ISO/FDIS 16000-33:2024(en)
International
Standard
ISO/FDIS 16000-33
ISO/TC 146/SC 6
Indoor air —
Secretariat: DIN
Part 33:
Voting begins on:
Determination of phthalates
with gas chromatography/mass
Voting terminates on:
spectrometry (GC/MS)
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.
© ISO 2024
IN ADDITION TO THEIR EVALUATION AS
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO-
LOGICAL, COMMERCIAL AND USER PURPOSES, DRAFT
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on
INTERNATIONAL STANDARDS MAY ON OCCASION HAVE
the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below
TO BE CONSIDERED IN THE LIGHT OF THEIR POTENTIAL
or ISO’s member body in the country of the requester.
TO BECOME STAN DARDS TO WHICH REFERENCE MAY BE
MADE IN NATIONAL REGULATIONS.
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 Reference number
ISO/FDIS 16000-33:2024(en) © ISO 2024
ii
ISO/FDIS 16000-33:2024(en)
Contents Page
Foreword .v
Introduction .vi
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Abbreviated terms . 2
5 Sampling methods and analytical apparatus. 3
5.1 General .3
5.2 Sampling by adsorption with subsequent thermal desorption .3
5.2.1 Apparatus, operating materials and chemicals .3
5.2.2 Preparation of the thermal desorption tube .4
5.2.3 Sampling .4
5.3 Sampling by adsorption and subsequent solvent extraction .5
5.3.1 Apparatus, operating materials and chemicals .5 ®
5.3.2 Preparation of Florisil and the adsorption tubes .6 ®
5.3.3 Suggestions regarding the application of Florisil .6
5.3.4 Sampling .7
5.3.5 Sample conditioning .7
6 Calibration . 8
6.1 General .8
6.2 Calibration of the thermal desorption method .8
6.3 Calibration of the solvent extraction method .8
7 Identification and quantification . 9
7.1 Mass spectrometric analysis .9
8 Establishment of calibration curves and calculation of the analyte mass. 14
8.1 Establishment of a calibration curve .14
8.2 Calculation of the analyte mass . .14
9 Calculation of indoor air concentrations .15
10 Performance characteristics . 16
10.1 Detection limit .16
10.2 Quantification limit and problems related to blank values .16
10.3 Reproducibility standard deviation and repeatability standard deviation .17
11 Quality assurance .18
11.1 Method verification and determination of blanks .18
11.1.1 General .18
11.1.2 Field blank value of the indoor air .18
11.1.3 Analytical laboratory blank value .19
11.2 Measures for blank value minimization .19
11.3 Documents.19
12 Interferences . 19
Annex A (informative) General information on phthalates .20
Annex B (informative) Sampling by adsorption with ODS solid phase disk or SDB copolymer
cartridge .23
Annex C (informative) Screening phthalates in solvent wipe tests .29
Annex D (informative) Screening phthalates in house dust .32
Annex E (informative) Practical example for the calibration of the thermal desorption method .36
iii
ISO/FDIS 16000-33:2024(en)
Annex F (informative) Practical example for the calibration of the solvent extraction method ®
using Florisil .38
Annex G (informative) Practical example for the gas chromatography with thermal desorption .40
Annex H (informative) Practical example for the gas chromatography following solvent
extraction . 41
Annex I (informative) Problems related to the blank values .42
Annex J (informative) Example of sampling protocol documentation .43
Bibliography .44
iv
ISO/FDIS 16000-33:2024(en)
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 document 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).
ISO draws attention to the possibility that the implementation of this document may involve the use of (a)
patent(s). ISO takes no position concerning the evidence, validity or applicability of any claimed patent
rights in respect thereof. As of the date of publication of this document, ISO had not received notice of (a)
patent(s) which may be required to implement this document. However, implementers are cautioned that
this may not represent the latest information, which may be obtained from the patent database available at
www.iso.org/patents. ISO shall not be held responsible for identifying any or all such patent rights.
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 146, Air quality, Subcommittee SC 6, Indoor air.
This second edition cancels and replaces the first edition (ISO 16000-33:2017), which has been technically
revised.
The main change is as follows: a descripti
...
ISO/FDIS 16000-33:2024(E)
ISO/TC 146/SC 6/WG 20
Secretariat: DIN
Date: 2024-02-23
Indoor air —
Part 33:
Determination of phthalates with gas chromatography/mass
spectrometry (GC-/MS)
Air intérieur —Partie 33: Détermination des phtalates par chromatographie en phase
gazeuse/spectrométrie de masse (CPG/SM)
Second edition
Date: 2023-12-04
ISO #####-#:####(X)
FDIS stage
2 © ISO #### – All rights reserved
ISO/FDIS 16000-33:2024(en)
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
EmailE-mail: copyright@iso.org
Website: www.iso.org
Published in Switzerland
iii
ISO/FDIS 16000-33:2024(en)
Contents
Foreword . vi
Introduction. vii
Part 33: Determination of phthalates with gas chromatography/mass spectrometry (GC/MS) .1
1 Scope .1
2 Normative references .1
3 Terms and definitions .1
4 Abbreviated terms .2
5 Sampling methods and analytical apparatus .4
5.1 General .4
5.2 Sampling by adsorption with subsequent thermal desorption .4
5.2.1 Apparatus, operating materials and chemicals .4
5.2.2 Preparation of the thermal desorption tube .5
5.2.3 Sampling .5
5.3 Sampling by adsorption and subsequent solvent extraction .6
5.3.1 Apparatus, operating materials and chemicals .6 ®
5.3.2 Preparation of Florisil and the adsorption tubes .7 ®
5.3.3 Suggestions regarding the application of Florisil .8
5.3.4 Sampling .8
5.3.5 Sample conditioning .9
6 Calibration .9
6.1 General .9
6.2 Calibration of the thermal desorption method . 10
6.3 Calibration of the solvent extraction method . 10
7 Identification and quantification . 10
7.1 Mass spectrometric analysis . 10
8 Establishment of calibration curves and calculation of the analyte mass . 17
8.1 Establishment of a calibration curve . 17
8.2 Calculation of the analyte mass . 18
9 Calculation of indoor air concentrations . 19
10 Performance characteristics . 20
10.1 Detection limit . 20
10.2 Quantification limit and problems related to blank values . 20
10.3 Reproducibility standard deviation and repeatability standard deviation . 21
11 Quality assurance . 22
11.1 Method verification and determination of blanks . 22
11.1.1 General . 22
11.1.2 Field blank value of the indoor air . 22
iv
ISO/FDIS 16000-33:2024(en)
11.1.3 Analytical laboratory blank value . 23
11.2 Measures for blank value minimization . 23
11.3 Documents . 23
12 Interferences . 23
Annex A (informative) General information on phthalates . 24
Annex B (informative) Sampling by adsorption with ODS solid phase disk or SDB copolymer cartridge . 28
Annex C (informative) Screening phthalates in solvent wipe tests . 35
Annex D (informative) Screening phthalates in house dust . 39
Annex E (informative) Practical example for the calibration of the thermal desorption method . 43 ®
Annex F (informative) Practical example for the calibration of the solvent extraction method using Florisil 45
Annex G (informative) Practical example for the gas chromatography with thermal desorption . 47
Annex H (informative) Practical example for the gas chromatography following solvent extraction . 48
Annex I (informative) Problems related to the blank values . 49
Annex J (informative) Example of sampling protocol documentation . 50
Bibliography . 51
v
ISO/FDIS 16000-33:2024(en)
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 document 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).
ISO draws attention to the possibility that the implementation of this document may involve the use of (a)
patent(s). ISO takes no position concerning the evidence, validity or applicability of any claimed patent rights
in respect thereof. As of the date of publication of this document, ISO had not received notice of (a) patent(s)
which may be required to implement this document. However, implementers are cautioned that this may not
represent the latest information, which may be obtained from the patent database available at
www.iso.org/patents. ISO shall not be held responsible for identifying any or all such patent rights.
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 146, Air quality, Subcommittee SC 6, Indoor air.
This second edition cancels and replaces the first edition (ISO 16000-33:2017), which has been technically
revised.
The main change is as follows: a description of an adsorbent which can alternatively be used has been added.
A list of all parts in the ISO 16000 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.
Field Code Changed
vi
ISO/FDIS 16000-33:2024(en)
Introduction
Different parts of the ISO 16000 series describe the general requirements relating to the measurement of
indoor air pollutants and the important conditions to be observed before or during the sampling of individual
pollutants or groups of pollutants, as well as the measurement procedures themselves.
The definition of indoor environment is given by ISO 16000-1. Dwellings [living rooms, bedrooms, do-it-
yourself (DIY) rooms, sports rooms and cellars, kitchens and bathrooms], workrooms or workplaces in
buildings which are not subject to health and safety inspections with respect to air pollutants (e.g. offices,
salesrooms), public buildings (e.g.,. restaurants, theatres, cinemas and other meeting rooms) and passenger
cabins of motor vehicles and public transport are among the most important types of indoor environment.
Phthalates, the diesters of the ortho-phthalic acid (1,2-benzene dicarboxylic acid), are emitted into the indoor
air primarily from articles of daily use made of soft polyvinyl chloride (PVC). Typically, phthalates are used as
plasticizers in soft PVC. Four most frequently used phthalates are diisodecylphthalate (DiDP),
diisononylphthalate (DiNP), di-2-ethylhexyl terephthalate (DOTP) and di-isononyl cyclohexane dicarboxylate
(DINCH but other families of esters are available. Di(2-ethylhexyl)-phthalate (DEHP), di-n-butyl-phthalate
(DBP),) and benzyl-n-butyl-phthalate (BBP) were used in Europe until more recent regulatory developments
placed restrictions on their use in the man
...
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