Indoor air

This document, along with ISO 16000-38, specifies the measurement method for determining the mass concentration of primary, secondary and tertiary aliphatic and aromatic amines in indoor air using accumulated sampling and high-performance liquid chromatography (HPLC) coupled with tandem mass spectrometry (MS-MS) or high-resolution mass spectrometry (HRMS). The analytical procedure is covered by this document. The sampling procedure and the manufacturing of the samplers are covered by ISO 16000-38. This document describes specifications for the chromatography and the mass spectroscopy for the amines. Measurement results are expressed in µg/m3. Although primarily intended for the measurement of amines listed in Tables A.1 and A.2, it can also be used for the measurement of other amines in indoor air. This document gives instructions and describes procedures for the inclusion of other amines. The range of application of this document concerning the concentrations of amines in indoor air depends on the linear range of the calibration line and hence on the gas sample volume (here: from 5 l up to 100 l), the eluate volume (from 1 ml up to 5 ml), the injection volume (from 1 µl up to 10 µl) and the sensitivity of the analytical equipment (e.g. linear range from 2 pg up to 2 ng amine). The range of application can be expected to be from approximately 0,002 µg/m3 (100 l sample) up to 2 000 µg/m3 (5 l sample) for a common analytical equipment (e.g. Waters ?TQD") for the majority of the amines listed in Tables A.1 and A.2. The analysis of derivatives of ethanolamine is usually about 10 times more sensitive and the analysis of short-chained aliphatic amines is usually about 10 times less sensitive than the analysis of an average amine. The performance data of the analytical method is given in Annex B, particularly in Tables B.1 and B.2. This document can be used also for the determination of amines in water if the detection limit is sufficient. This document does not cover the determination of isocyanates in indoor air (nor in water samples) as corresponding amines (covered by ISO 17734-1 and ISO 17734-2).

Air intérieur

Notranji zrak - 39. del: Določevanje aminov - Analiza aminov s tekočinsko kromatografijo visoke ločljivosti (HPLC), sklopljeno z masno spektrometrijo visoke ločljivosti (HRMS) ali tandemsko masno spektrometrijo (MS-MS)

Ta dokument, skupaj s standardom ISO 16000-38, določa metodo merjenja masne koncentracije primarnih, sekundarnih in terciarnih alifatskih ter aromatskih aminov v notranjem zraku z uporabo akumuliranega vzorčenja in visokozmogljive tekočinske kromatografije (HPLC) skupaj s tandemsko masno spektrometrijo (MS-MS) ali masno spektrometrijo visoke ločljivosti (HRMS). Dokument zajema analitični postopek. Postopek vzorčenja in izdelava vzorčevalnikov sta zajeta v standardu ISO 16000-38. Ta dokument opisuje specifikacije za kromatografijo in masno spektroskopijo aminov. Rezultati meritev so izraženi v μg/m3. Čeprav je dokument namenjen predvsem za merjenje aminov, naštetih v dodatku A.1 in A.2, se lahko uporablja tudi za merjenje drugih aminov v notranjem zraku. Dokument vsebuje navodila in opisuje postopke za vključitev drugih aminov. Področje uporabe tega dokumenta v zvezi s koncentracijami aminov v notranjem zraku je odvisno od linearnega obsega kalibracijske krivulje in s tem od volumna vzorca plina (tukaj: od 5 l do 100 l), volumna eluata (od 1 ml do 5 ml), volumna vbrizgavanja (od 1 μl do 10 μl) in občutljivosti analitične opreme (npr. linearni razpon od 2 pg do 2 ng amina). Področje uporabe je mogoče pričakovati od približno 0,002 μg/m3 (vzorec 100 l) do 2000 μg/m3 (vzorec 5 l) za skupno analitsko opremo (npr. vode »TQD«) za večino aminov iz preglednic A.1 in A.2. Analiza derivatov etanolamina je običajno približno 10-krat občutljivejša, analiza kratko verižnih alifatskih aminov pa je običajno približno 10-krat manj občutljiva kot
analiza povprečnega amina. Podatki o učinkovitosti analitske metode so navedeni v dodatku B, zlasti v preglednicah B.1 in B.2. Ta dokument je mogoče uporabiti tudi za določanje aminov v vodi, če je meja zaznavanja zadostna. Ta dokument ne zajema določevanja izocianatov kot ustreznih aminov v notranjem zraku (niti v vzorcih vode) (zajeto v standardih ISO 17734-1 in ISO 17734-2).

General Information

Status
Published
Publication Date
30-May-2019
Technical Committee
Drafting Committee
Current Stage
6060 - International Standard published
Start Date
02-May-2019
Completion Date
31-May-2019

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INTERNATIONAL ISO
STANDARD 16000-39
First edition
2019-06
Indoor air —
Part 39:
Determination of amines —
Analysis of amines by (ultra-) high-
performance liquid chromatography
coupled to high resolution or tandem
mass spectrometry
Reference number
ISO 16000-39:2019(E)
ISO 2019
---------------------- Page: 1 ----------------------
ISO 16000-39:2019(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2019

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
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2019 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 16000-39:2019(E)
Contents Page

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

Introduction ..................................................................................................................................................................................................................................v

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

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

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

4 Amines in indoor air ......................................................................................................................................................................................... 2

4.1 Properties of amines .......................................................................................................................................................................... 2

4.2 Origin and occurrence of amines ............................................................................................................................................ 2

5 Analytical procedure ........................................................................................................................................................................................ 2

5.1 Preparation of sample solutions .............................................................................................................................................. 2

5.2 High-performance liquid chromatography .................................................................................................................... 2

5.3 Tandem mass spectrometry ........................................................................................................................................................ 3

5.4 High resolution mass spectrometry ..................................................................................................................................... 3

5.5 Sample sequence and external calibration ..................................................................................................................... 3

6 Testing of the suitability of the equipment and the instrumental analysis ............................................3

6.1 General ........................................................................................................................................................................................................... 3

6.2 High-performance or ultra-performance liquid chromatography (HPLC or UHPLC) ............... 3

6.3 Tandem mass spectrometry (MS-MS) ................................................................................................................................. 4

6.4 High resolution mass spectrometry (HRMS) ................................................................................................................ 4

7 Reporting requirements ............................................................................................................................................................................... 4

Annex A (informative) List of included amines ......................................................................................................................................... 6

Annex B (informative) Performance data of the analytical method .................................................................................... 9

Bibliography .............................................................................................................................................................................................................................12

© ISO 2019 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 16000-39:2019(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 146, Air quality, Subcommittee SC 6,

Indoor air.
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.
iv © ISO 2019 – All rights reserved
---------------------- Page: 4 ----------------------
ISO 16000-39:2019(E)
Introduction

ISO 16000 (all parts) describe 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 measurements procedures themselves.

The definition of indoor environment is given by ISO 16000-1. Dwellings [living rooms, bedrooms, do-

it-yourself (DIY) rooms, sport 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 transportation are among the most important types of

indoor environment.
© ISO 2019 – All rights reserved v
---------------------- Page: 5 ----------------------
INTERNATIONAL STANDARD ISO 16000-39:2019(E)
Indoor air —
Part 39:
Determination of amines — Analysis of amines by (ultra-)
high-performance liquid chromatography coupled to high
resolution or tandem mass spectrometry
1 Scope

This document, along with ISO 16000-38, specifies the measurement method for determining the mass

concentration of primary, secondary and tertiary aliphatic and aromatic amines in indoor air using

accumulated sampling and high-performance liquid chromatography (HPLC) coupled with tandem

mass spectrometry (MS-MS) or high-resolution mass spectrometry (HRMS). The analytical procedure

is covered by this document. The sampling procedure and the manufacturing of the samplers are

covered by ISO 16000-38.

This document describes specifications for the chromatography and the mass spectroscopy for the

amines. Measurement results are expressed in µg/m .

Although primarily intended for the measurement of amines listed in Tables A.1 and A.2, it can also be

used for the measurement of other amines in indoor air. This document gives instructions and describes

procedures for the inclusion of other amines.

The range of application of this document concerning the concentrations of amines in indoor air

depends on the linear range of the calibration line and hence on the gas sample volume (here: from 5 l

up to 100 l), the eluate volume (from 1 ml up to 5 ml), the injection volume (from 1 µl up to 10 µl) and

the sensitivity of the analytical equipment (e.g. linear range from 2 pg up to 2 ng amine). The range

of application can be expected to be from approximately 0,002 µg/m (100 l sample) up to 2 000 µg/

m (5 l sample) for a common analytical equipment (e.g. Waters „TQD“) for the majority of the amines

listed in Tables A.1 and A.2. The analysis of derivatives of ethanolamine is usually about 10 times more

sensitive and the analysis of short-chained aliphatic amines is usually about 10 times less sensitive than

the analysis of an average amine.

The performance data of the analytical method is given in Annex B, particularly in Tables B.1 and B.2.

This document can be used also for the determination of amines in water if the detection limit is

sufficient.

This document does not cover the determination of isocyanates in indoor air (nor in water samples) as

corresponding amines (covered by ISO 17734-1 and ISO 17734-2).
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 16000-38, Indoor air — Part 38: Determination of amines in indoor and test chamber air — Active

sampling on samplers containing phosphoric acid impregnated filters
© ISO 2019 – All rights reserved 1
---------------------- Page: 6 ----------------------
ISO 16000-39:2019(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 standardisation at the following addresses:

— ISO online browsing platform: available at http: //www .iso .org/obp
— IEC Electropedia: aivailable at http: //www .elctropedia .org/
3.1
amines

nitrogen containing compounds with a sufficient vapor pressure (>10 Pa) and a free electron pair at

the nitrogen atom which can be protonated
4 Amines in indoor air
4.1 Properties of amines
Amines are basic and polar substances.
There are primary, secondary, tertiary, and quaternary amines.

Quaternary amines are not included in this document, as they have no free electron pair and therefore

have very different properties. In this document the term “amines” refers only to primary, secondary,

and tertiary amines.
Not protonated amines are oxidation sensitive.

Reaction of amines with acids results in ammonium salts of the amines. The ammonium salts are not

oxidation sensitive.
4.2 Origin and occurrence of amines

Amines are produced by technical chemical processes and processing and in addition by biotic or

abiotic decomposition of nitrogen compounds. Besides sources of biological origin, indoor air sources of

amines could be, for instance, products containing polyurethane, especially foams, e.g. in vehicle seats,

mattresses, pillows, and upholstered furniture or as thermal insulation or sound absorbing material.

Several amines, in particular aromatic amines, are known as harmful compounds. Furthermore, most

amines have an unacceptable odour in combination with a low odour threshold.

Further sources are for example food, e.g. fish (aliphatic amines), and cigarette smoke (aromatic

amines).
5 Analytical procedure
5.1 Preparation of sample solutions

ISO 16000-38 describes the procedure to get the aqueous eluate of the ammonium salts of the sampled

amines. The sample solution (which contains already approximately 0,02 µmol/µl up to 0,1 µmol/µl

phosphoric acid) can be used for the injection into the HPLC system without further treatment.

5.2 High-performance liquid chromatography
— stationary phase of separating column: pentafluorophenyl;
— common column dimensions: length 150 mm, inner diameter: 2,1 mm;
2 © ISO 2019 – All rights reserved
---------------------- Page: 7 ----------------------
ISO 16000-39:2019(E)

— common particle size: 3 μm (HPLC), 1,7 µm [Ultra Performance Liquid Chromatography (UHPLC)];

— column temperature: 40 °C;
— injection volume: 1 µl to 10 μl;

— mobile phase: acetonitrile and water with each 0,02 % formic acid (500 µl formic acid in 2,5 l

acetonitrile or 2,5 l water, respectively);
— mobile phase composition: 28 % acetonitrile/72 % water, isocratic.
5.3 Tandem mass spectrometry
— ionisation: electrospray ionisation, positive mode (ESI );
— source temperature: 120 °C;
— desolvation gas: nitrogen, 900 l/h;
— desolvation temperature: 420 °C;
— cone gas: nitrogen, 50 l/h;
— precursor ion: M+1;
— collision gas: argon;
— calibration: external and additionally with Pyridine-d5 as internal standard.
5.4 High resolution mass spectrometry
— ionisation: electrospray ionisation, positive mode (ESI ).
5.5 Sample sequence and external calibration

— external calibration: run calibration standards at least at the beginning and at the end of a sample

sequence;

— every 25 samples or less and at the beginning and end, run a calibration blank and a calibration

check solution of an independent source;

— every 50 samples (for example) and at the end of a run, analyse an interference check solution (ICS).

6 Testing of the suitability of the equipment and the instrumental analysis
6.1 General

In Table A.3, several amines are listed which can interfere with another amine in the instrumental

analysis. In order to check and confirm the suitability of the selected system and procedure following

issues have to be tested.
6.2 High-performance or ultra-performance liquid chromatography (HPLC or UHPLC)

The chromatographic separation of following compounds has to be tested and confirmed:

a) Diethylamine (11) and N,N-Dimethylethylamine (24);
b) Isobutylamine (2) and n-Butylamine (10);
c) 2-(Dimethylamino)ethanol (8) and 2-(Ethylamino)ethanol (25);
© ISO 2019 – All rights reserved 3
---------------------- Page: 8 ----------------------
ISO 16000-39:2019(E)
d) Diisobutylamine (14) and Di-n-butylamin (16).

Usually 4-Ethylmorpholine (4) and 2-(Diethylamino)ethanol (3) as well as Morpholine (13) and

2-(Dimethylamino)ethanol (8) cannot be separated sufficiently on pentafluorphenyl terminated

stationary phases. These compounds have to be distinguished by high resolution or tandem mass

spectrometry.

The chromatographic separation of Diethylamine (11) and N,N-Dimethylethylamine (24) is not always

possible (depends mainly on the column). If tandem mass spectrometry is used for detection the ratio

of the product ions (46 a
...

SLOVENSKI STANDARD
SIST ISO 16000-39:2019
01-december-2019
Notranji zrak - 39. del: Določevanje aminov - Analiza aminov s tekočinsko

kromatografijo visoke ločljivosti (HPLC), sklopljeno z masno spektrometrijo visoke

ločljivosti (HRMS) ali tandemsko masno spektrometrijo (MS-MS)

Indoor air - Part 39: Determination of amines - Analysis of amines by (ultra-) high-

performance liquid chromatography coupled to high resolution or tandem mass
spectrometry
Ta slovenski standard je istoveten z: ISO 16000-39:2019
ICS:
13.040.20 Kakovost okoljskega zraka Ambient atmospheres
SIST ISO 16000-39:2019 en

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
SIST ISO 16000-39:2019
---------------------- Page: 2 ----------------------
SIST ISO 16000-39:2019
INTERNATIONAL ISO
STANDARD 16000-39
First edition
2019-06
Indoor air —
Part 39:
Determination of amines —
Analysis of amines by (ultra-) high-
performance liquid chromatography
coupled to high resolution or tandem
mass spectrometry
Reference number
ISO 16000-39:2019(E)
ISO 2019
---------------------- Page: 3 ----------------------
SIST ISO 16000-39:2019
ISO 16000-39:2019(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2019

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
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2019 – All rights reserved
---------------------- Page: 4 ----------------------
SIST ISO 16000-39:2019
ISO 16000-39:2019(E)
Contents Page

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

Introduction ..................................................................................................................................................................................................................................v

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

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

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

4 Amines in indoor air ......................................................................................................................................................................................... 2

4.1 Properties of amines .......................................................................................................................................................................... 2

4.2 Origin and occurrence of amines ............................................................................................................................................ 2

5 Analytical procedure ........................................................................................................................................................................................ 2

5.1 Preparation of sample solutions .............................................................................................................................................. 2

5.2 High-performance liquid chromatography .................................................................................................................... 2

5.3 Tandem mass spectrometry ........................................................................................................................................................ 3

5.4 High resolution mass spectrometry ..................................................................................................................................... 3

5.5 Sample sequence and external calibration ..................................................................................................................... 3

6 Testing of the suitability of the equipment and the instrumental analysis ............................................3

6.1 General ........................................................................................................................................................................................................... 3

6.2 High-performance or ultra-performance liquid chromatography (HPLC or UHPLC) ............... 3

6.3 Tandem mass spectrometry (MS-MS) ................................................................................................................................. 4

6.4 High resolution mass spectrometry (HRMS) ................................................................................................................ 4

7 Reporting requirements ............................................................................................................................................................................... 4

Annex A (informative) List of included amines ......................................................................................................................................... 6

Annex B (informative) Performance data of the analytical method .................................................................................... 9

Bibliography .............................................................................................................................................................................................................................12

© ISO 2019 – All rights reserved iii
---------------------- Page: 5 ----------------------
SIST ISO 16000-39:2019
ISO 16000-39:2019(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 146, Air quality, Subcommittee SC 6,

Indoor air.
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.
iv © ISO 2019 – All rights reserved
---------------------- Page: 6 ----------------------
SIST ISO 16000-39:2019
ISO 16000-39:2019(E)
Introduction

ISO 16000 (all parts) describe 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 measurements procedures themselves.

The definition of indoor environment is given by ISO 16000-1. Dwellings [living rooms, bedrooms, do-

it-yourself (DIY) rooms, sport 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 transportation are among the most important types of

indoor environment.
© ISO 2019 – All rights reserved v
---------------------- Page: 7 ----------------------
SIST ISO 16000-39:2019
---------------------- Page: 8 ----------------------
SIST ISO 16000-39:2019
INTERNATIONAL STANDARD ISO 16000-39:2019(E)
Indoor air —
Part 39:
Determination of amines — Analysis of amines by (ultra-)
high-performance liquid chromatography coupled to high
resolution or tandem mass spectrometry
1 Scope

This document, along with ISO 16000-38, specifies the measurement method for determining the mass

concentration of primary, secondary and tertiary aliphatic and aromatic amines in indoor air using

accumulated sampling and high-performance liquid chromatography (HPLC) coupled with tandem

mass spectrometry (MS-MS) or high-resolution mass spectrometry (HRMS). The analytical procedure

is covered by this document. The sampling procedure and the manufacturing of the samplers are

covered by ISO 16000-38.

This document describes specifications for the chromatography and the mass spectroscopy for the

amines. Measurement results are expressed in µg/m .

Although primarily intended for the measurement of amines listed in Tables A.1 and A.2, it can also be

used for the measurement of other amines in indoor air. This document gives instructions and describes

procedures for the inclusion of other amines.

The range of application of this document concerning the concentrations of amines in indoor air

depends on the linear range of the calibration line and hence on the gas sample volume (here: from 5 l

up to 100 l), the eluate volume (from 1 ml up to 5 ml), the injection volume (from 1 µl up to 10 µl) and

the sensitivity of the analytical equipment (e.g. linear range from 2 pg up to 2 ng amine). The range

of application can be expected to be from approximately 0,002 µg/m (100 l sample) up to 2 000 µg/

m (5 l sample) for a common analytical equipment (e.g. Waters „TQD“) for the majority of the amines

listed in Tables A.1 and A.2. The analysis of derivatives of ethanolamine is usually about 10 times more

sensitive and the analysis of short-chained aliphatic amines is usually about 10 times less sensitive than

the analysis of an average amine.

The performance data of the analytical method is given in Annex B, particularly in Tables B.1 and B.2.

This document can be used also for the determination of amines in water if the detection limit is

sufficient.

This document does not cover the determination of isocyanates in indoor air (nor in water samples) as

corresponding amines (covered by ISO 17734-1 and ISO 17734-2).
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 16000-38, Indoor air — Part 38: Determination of amines in indoor and test chamber air — Active

sampling on samplers containing phosphoric acid impregnated filters
© ISO 2019 – All rights reserved 1
---------------------- Page: 9 ----------------------
SIST ISO 16000-39:2019
ISO 16000-39:2019(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 standardisation at the following addresses:

— ISO online browsing platform: available at http: //www .iso .org/obp
— IEC Electropedia: aivailable at http: //www .elctropedia .org/
3.1
amines

nitrogen containing compounds with a sufficient vapor pressure (>10 Pa) and a free electron pair at

the nitrogen atom which can be protonated
4 Amines in indoor air
4.1 Properties of amines
Amines are basic and polar substances.
There are primary, secondary, tertiary, and quaternary amines.

Quaternary amines are not included in this document, as they have no free electron pair and therefore

have very different properties. In this document the term “amines” refers only to primary, secondary,

and tertiary amines.
Not protonated amines are oxidation sensitive.

Reaction of amines with acids results in ammonium salts of the amines. The ammonium salts are not

oxidation sensitive.
4.2 Origin and occurrence of amines

Amines are produced by technical chemical processes and processing and in addition by biotic or

abiotic decomposition of nitrogen compounds. Besides sources of biological origin, indoor air sources of

amines could be, for instance, products containing polyurethane, especially foams, e.g. in vehicle seats,

mattresses, pillows, and upholstered furniture or as thermal insulation or sound absorbing material.

Several amines, in particular aromatic amines, are known as harmful compounds. Furthermore, most

amines have an unacceptable odour in combination with a low odour threshold.

Further sources are for example food, e.g. fish (aliphatic amines), and cigarette smoke (aromatic

amines).
5 Analytical procedure
5.1 Preparation of sample solutions

ISO 16000-38 describes the procedure to get the aqueous eluate of the ammonium salts of the sampled

amines. The sample solution (which contains already approximately 0,02 µmol/µl up to 0,1 µmol/µl

phosphoric acid) can be used for the injection into the HPLC system without further treatment.

5.2 High-performance liquid chromatography
— stationary phase of separating column: pentafluorophenyl;
— common column dimensions: length 150 mm, inner diameter: 2,1 mm;
2 © ISO 2019 – All rights reserved
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SIST ISO 16000-39:2019
ISO 16000-39:2019(E)

— common particle size: 3 μm (HPLC), 1,7 µm [Ultra Performance Liquid Chromatography (UHPLC)];

— column temperature: 40 °C;
— injection volume: 1 µl to 10 μl;

— mobile phase: acetonitrile and water with each 0,02 % formic acid (500 µl formic acid in 2,5 l

acetonitrile or 2,5 l water, respectively);
— mobile phase composition: 28 % acetonitrile/72 % water, isocratic.
5.3 Tandem mass spectrometry
— ionisation: electrospray ionisation, positive mode (ESI );
— source temperature: 120 °C;
— desolvation gas: nitrogen, 900 l/h;
— desolvation temperature: 420 °C;
— cone gas: nitrogen, 50 l/h;
— precursor ion: M+1;
— collision gas: argon;
— calibration: external and additionally with Pyridine-d5 as internal standard.
5.4 High resolution mass spectrometry
— ionisation: electrospray ionisation, positive mode (ESI ).
5.5 Sample sequence and external calibration

— external calibration: run calibration standards at least at the beginning and at the end of a sample

sequence;

— every 25 samples or less and at the beginning and end, run a calibration blank and a calibration

check solution of an independent source;

— every 50 samples (for example) and at the end of a run, analyse an interference check solution (ICS).

6 Testing of the suitability of the equipment and the instrumental analysis
6.1 General

In Table A.3, several amines are listed which can interfere with another amine in the instrumental

analysis. In order to check and confirm the suitability of the selected system and procedure following

issues have to be tested.
6.2 High-performance or ultra-performance liquid chromatography (HPLC or UHPLC)

The chromatographic separation of following compounds has to be tested and confirmed:

a) Diethylamine (11) and N,N-Dimethylethylamine (24);
b) Isobutylamine (2) and n-Butylamine (10);
c) 2-(Dimethylamino)ethanol (8) and 2-(Ethylamino)ethanol (25);
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SIST ISO 16000-39:2019
ISO 16000-39:2019(E)
d) Diisobutylamine (
...

SLOVENSKI STANDARD
oSIST ISO 16000-39:2019
01-september-2019
Notranji zrak - 39. del: Določevanje aminov - Analiza aminov s tekočinsko

kromatografijo visoke ločljivosti (HPLC), sklopljeno z masno spektrometrijo visoke

ločljivosti (HRMS) ali tandemsko masno spektrometrijo (MS-MS)

Indoor air - Part 39: Determination of amines - Analysis of amines by (ultra-) high-

performance liquid chromatography coupled to high resolution or tandem mass
spectrometry
Ta slovenski standard je istoveten z: ISO 16000-39:2019
ICS:
13.040.20 Kakovost okoljskega zraka Ambient atmospheres
oSIST ISO 16000-39:2019 en

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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oSIST ISO 16000-39:2019
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oSIST ISO 16000-39:2019
INTERNATIONAL ISO
STANDARD 16000-39
First edition
2019-06
Indoor air —
Part 39:
Determination of amines —
Analysis of amines by (ultra-) high-
performance liquid chromatography
coupled to high resolution or tandem
mass spectrometry
Reference number
ISO 16000-39:2019(E)
ISO 2019
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oSIST ISO 16000-39:2019
ISO 16000-39:2019(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2019

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
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2019 – All rights reserved
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oSIST ISO 16000-39:2019
ISO 16000-39:2019(E)
Contents Page

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

Introduction ..................................................................................................................................................................................................................................v

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

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

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

4 Amines in indoor air ......................................................................................................................................................................................... 2

4.1 Properties of amines .......................................................................................................................................................................... 2

4.2 Origin and occurrence of amines ............................................................................................................................................ 2

5 Analytical procedure ........................................................................................................................................................................................ 2

5.1 Preparation of sample solutions .............................................................................................................................................. 2

5.2 High-performance liquid chromatography .................................................................................................................... 2

5.3 Tandem mass spectrometry ........................................................................................................................................................ 3

5.4 High resolution mass spectrometry ..................................................................................................................................... 3

5.5 Sample sequence and external calibration ..................................................................................................................... 3

6 Testing of the suitability of the equipment and the instrumental analysis ............................................3

6.1 General ........................................................................................................................................................................................................... 3

6.2 High-performance or ultra-performance liquid chromatography (HPLC or UHPLC) ............... 3

6.3 Tandem mass spectrometry (MS-MS) ................................................................................................................................. 4

6.4 High resolution mass spectrometry (HRMS) ................................................................................................................ 4

7 Reporting requirements ............................................................................................................................................................................... 4

Annex A (informative) List of included amines ......................................................................................................................................... 6

Annex B (informative) Performance data of the analytical method .................................................................................... 9

Bibliography .............................................................................................................................................................................................................................12

© ISO 2019 – All rights reserved iii
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oSIST ISO 16000-39:2019
ISO 16000-39:2019(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 146, Air quality, Subcommittee SC 6,

Indoor air.
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.
iv © ISO 2019 – All rights reserved
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oSIST ISO 16000-39:2019
ISO 16000-39:2019(E)
Introduction

ISO 16000 (all parts) describe 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 measurements procedures themselves.

The definition of indoor environment is given by ISO 16000-1. Dwellings [living rooms, bedrooms, do-

it-yourself (DIY) rooms, sport 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 transportation are among the most important types of

indoor environment.
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oSIST ISO 16000-39:2019
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oSIST ISO 16000-39:2019
INTERNATIONAL STANDARD ISO 16000-39:2019(E)
Indoor air —
Part 39:
Determination of amines — Analysis of amines by (ultra-)
high-performance liquid chromatography coupled to high
resolution or tandem mass spectrometry
1 Scope

This document, along with ISO 16000-38, specifies the measurement method for determining the mass

concentration of primary, secondary and tertiary aliphatic and aromatic amines in indoor air using

accumulated sampling and high-performance liquid chromatography (HPLC) coupled with tandem

mass spectrometry (MS-MS) or high-resolution mass spectrometry (HRMS). The analytical procedure

is covered by this document. The sampling procedure and the manufacturing of the samplers are

covered by ISO 16000-38.

This document describes specifications for the chromatography and the mass spectroscopy for the

amines. Measurement results are expressed in µg/m .

Although primarily intended for the measurement of amines listed in Tables A.1 and A.2, it can also be

used for the measurement of other amines in indoor air. This document gives instructions and describes

procedures for the inclusion of other amines.

The range of application of this document concerning the concentrations of amines in indoor air

depends on the linear range of the calibration line and hence on the gas sample volume (here: from 5 l

up to 100 l), the eluate volume (from 1 ml up to 5 ml), the injection volume (from 1 µl up to 10 µl) and

the sensitivity of the analytical equipment (e.g. linear range from 2 pg up to 2 ng amine). The range

of application can be expected to be from approximately 0,002 µg/m (100 l sample) up to 2 000 µg/

m (5 l sample) for a common analytical equipment (e.g. Waters „TQD“) for the majority of the amines

listed in Tables A.1 and A.2. The analysis of derivatives of ethanolamine is usually about 10 times more

sensitive and the analysis of short-chained aliphatic amines is usually about 10 times less sensitive than

the analysis of an average amine.

The performance data of the analytical method is given in Annex B, particularly in Tables B.1 and B.2.

This document can be used also for the determination of amines in water if the detection limit is

sufficient.

This document does not cover the determination of isocyanates in indoor air (nor in water samples) as

corresponding amines (covered by ISO 17734-1 and ISO 17734-2).
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 16000-38, Indoor air — Part 38: Determination of amines in indoor and test chamber air — Active

sampling on samplers containing phosphoric acid impregnated filters
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oSIST ISO 16000-39:2019
ISO 16000-39:2019(E)
3 Terms a nd definiti ons
For the purposes of this document, the following terms and definitions apply.

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

— ISO online browsing platform: available at http: //www .iso .org/obp
— IEC Electropedia: aivailable at http: //www .elctropedia .org/
3.1
amines

nitrogen containing compounds with a sufficient vapor pressure (>10 Pa) and a free electron pair at

the nitrogen atom which can be protonated
4 Amines in indoor air
4.1 Properties of amines
Amines are basic and polar substances.
There are primary, secondary, tertiary, and quaternary amines.

Quaternary amines are not included in this document, as they have no free electron pair and therefore

have very different properties. In this document the term “amines” refers only to primary, secondary,

and tertiary amines.
Not protonated amines are oxidation sensitive.

Reaction of amines with acids results in ammonium salts of the amines. The ammonium salts are not

oxidation sensitive.
4.2 Origin and occurrence of amines

Amines are produced by technical chemical processes and processing and in addition by biotic or

abiotic decomposition of nitrogen compounds. Besides sources of biological origin, indoor air sources of

amines could be, for instance, products containing polyurethane, especially foams, e.g. in vehicle seats,

mattresses, pillows, and upholstered furniture or as thermal insulation or sound absorbing material.

Several amines, in particular aromatic amines, are known as harmful compounds. Furthermore, most

amines have an unacceptable odour in combination with a low odour threshold.

Further sources are for example food, e.g. fish (aliphatic amines), and cigarette smoke (aromatic

amines).
5 Analytical procedure
5.1 Preparation of sample solutions

ISO 16000-38 describes the procedure to get the aqueous eluate of the ammonium salts of the sampled

amines. The sample solution (which contains already approximately 0,02 µmol/µl up to 0,1 µmol/µl

phosphoric acid) can be used for the injection into the HPLC system without further treatment.

5.2 High-performance liquid chromatography
— stationary phase of separating column: pentafluorophenyl;
— common column dimensions: length 150 mm, inner diameter: 2,1 mm;
2 © ISO 2019 – All rights reserved
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oSIST ISO 16000-39:2019
ISO 16000-39:2019(E)

— common particle size: 3 μm (HPLC), 1,7 µm [Ultra Performance Liquid Chromatography (UHPLC)];

— column temperature: 40 °C;
— injection volume: 1 µl to 10 μl;

— mobile phase: acetonitrile and water with each 0,02 % formic acid (500 µl formic acid in 2,5 l

acetonitrile or 2,5 l water, respectively);
— mobile phase composition: 28 % acetonitrile/72 % water, isocratic.
5.3 Tandem mass spectrometry
— ionisation: electrospray ionisation, positive mode (ESI );
— source temperature: 120 °C;
— desolvation gas: nitrogen, 900 l/h;
— desolvation temperature: 420 °C;
— cone gas: nitrogen, 50 l/h;
— precursor ion: M+1;
— collision gas: argon;
— calibration: external and additionally with Pyridine-d5 as internal standard.
5.4 High resolution mass spectrometry
— ionisation: electrospray ionisation, positive mode (ESI ).
5.5 Sample sequence and external calibration

— external calibration: run calibration standards at least at the beginning and at the end of a sample

sequence;

— every 25 samples or less and at the beginning and end, run a calibration blank and a calibration

check solution of an independent source;

— every 50 samples (for example) and at the end of a run, analyse an interference check solution (ICS).

6 Testing of the suitability of the equipment and the instrumental analysis
6.1 General

In Table A.3, several amines are listed which can interfere with another amine in the instrumental

analysis. In order to check and confirm the suitability of the selected system and procedure following

issues have to be tested.
6.2 High-performance or ultra-performance liquid chromatography (HPLC or UHPLC)

The chromatographic separation of following compounds has to be tested and confirmed:

a) Diethylamine (11) and N,N-Dimethylethylamine (24);
b) Isobutylamine (2) and n-Butylamine (10);
c) 2-(Dimethylamino)ethanol (8) and 2-(Ethylamino)ethanol (25);
© ISO 2019 – All rights reserved 3
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oSIST ISO 16000-39:2019
ISO 16000-39:2019(E)
d) Diisobutylamine (14) and Di-n-butylamin (16).
...

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