Indoor air

Air intérieur

Notranji zrak - 6. del: Določevanje hlapnih organskih spojin (VVOC, VOC, SVOC) v notranjem zraku in zraku v preskusnih komorah z aktivnim vzorčenjem v cevkah z adsorpcijskim polnilom, termično desorpcijo in plinsko kromatografijo z MS ali MS-FID

General Information

Status

Published

ICS

13.040.20 - Ambient atmospheres

Technical Committee

ISO/TC 146/SC 6 - Indoor air

Drafting Committee

ISO/TC 146/SC 6/WG 3 - Determination of volatile organic compounds (VOCs) in indoor air

Current Stage

5020 - FDIS ballot initiated: 2 months. Proof sent to secretariat

Start Date

05-May-2021

Completion Date

05-May-2021

Ref Project

kSIST ISO/FDIS 16000-6:2021 - Indoor air - Part 6: Determination of organic compounds (VVOC, VOC, SVOC) in indoor and test chamber air by active sampling on sorbent tubes, thermal desorption and gas chromatography using MS or MS FID

RELATIONS

Revised

ISO 16000-6:2011 - Indoor air

Effective Date

01-Apr-2017

Buy Standard

Draft

ISO/FDIS 16000-6 - Indoor air

English language

37 pages

sale 15% off

Preview

sale 15% off

Preview

Draft

ISO/DIS 16000-6:2021

English language

41 pages

sale 10% off

Preview

sale 10% off

Preview

e-Library read for

1 day

Draft

ISO/FDIS 16000-6 - Air intérieur

French language

39 pages

sale 15% off

Preview

sale 15% off

Preview

Standards Content (sample)

FINAL
INTERNATIONAL ISO/FDIS
DRAFT
STANDARD 16000-6
ISO/TC 146/SC 6
Indoor air —
Secretariat: DIN
Voting begins on:
Part 6:
2021-05-05
Determination of organic compounds
Voting terminates on:
(VVOC, VOC, SVOC) in indoor and test
2021-06-30
chamber air by active sampling on
sorbent tubes, thermal desorption and
gas chromatography using MS or MS
FID
Air intérieur —
Partie 6: Dosage des composés organiques (COTV, COV, COSV) dans
l'air intérieur et l'air de chambre d'essai par prélèvement actif sur
tubes à sorbant, désorption thermique et chromatographie en phase
gazeuse avec détection MS ou MS-FID
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 16000-6:2021(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 2021
---------------------- Page: 1 ----------------------
ISO/FDIS 16000-6:2021(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2021

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/FDIS 16000-6:2021(E)
Contents Page

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

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

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

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

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

4 Abbreviated terms .............................................................................................................................................................................................. 3

5 Principle ........................................................................................................................................................................................................................ 3

6 Reagents and materials ................................................................................................................................................................................. 3

7 Apparatus ..................................................................................................................................................................................................................... 5

8 Conditioning and storage of sorbent tubes ............................................................................................................................... 9

8.1 Conditioning .............................................................................................................................................................................................. 9

8.2 Storage of conditioned sorbent tubes before sampling ....................................................................................10

9 Sampling .....................................................................................................................................................................................................................10

9.1 Air sampling ...........................................................................................................................................................................................10

9.2 Sampling volumes .............................................................................................................................................................................10

9.3 Storage of loaded samples..........................................................................................................................................................11

9.4 Field blanks .............................................................................................................................................................................................11

10 Analysis .......................................................................................................................................................................................................................11

10.1 Determination of VOC, VVOC and SVOC ..........................................................................................................................11

10.1.1 Analytical System .........................................................................................................................................................11

10.1.2 Identification of target compounds ..............................................................................................................13

10.1.3 Quantification of target compounds and compounds according to task list ............14

10.1.4 Determining the lower limit of quantification ....................................................................................16

10.2 Identified non-target compounds and unidentified compounds .............................................................16

11 Concentration of analytes in the sampled air ......................................................................................................................16

12 Performance characteristics .................................................................................................................................................................17

13 Test report ................................................................................................................................................................................................................18

14 Quality control .....................................................................................................................................................................................................19

Annex A (informative) Total volatile organic compounds (TVOC) and total semi-volatile

organic compounds (TSVOC) ................................................................................................................................................................20

Annex B (informative) Examples of compounds detected in indoor air and from building

products in test chambers .......................................................................................................................................................................22

Annex C (informative) Description of sorbents ......................................................................................................................................28

Annex D (informative) Guide on sorbent usage .....................................................................................................................................29

Annex E (informative) Safe sampling volumes for selected organic vapours .........................................................31

Annex F (informative) Storage recovery of solvents on sorbent tubes ..........................................................................34

Bibliography .............................................................................................................................................................................................................................36

© ISO 2021 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO/FDIS 16000-6:2021(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 146 Air quality, Subcommittee SC 6,

Indoor air.

This third edition cancels and replaces the second edition (ISO 16000-6:2012), which has been

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

— other sorbents than Tenax TA are allowed to be used;

— descriptions of VVOC and SVOC measurements are included in the mandatory part of the document.

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 2021 – All rights reserved
---------------------- Page: 4 ----------------------
ISO/FDIS 16000-6:2021(E)
Introduction

ISO 16000-1 establishes 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. Aspects of the determination (sampling and analysis) and the sampling strategy

of specific pollutants or groups of pollutants are specified in the subsequent parts of ISO 16000 (see

Foreword).

ISO 16000-5 (dealing with VOC sampling strategy) is a link between ISO 16000-1 (a generic standard

establishing the principles) and this part of ISO 16000, which deals with sampling and analytical

measurements.
[3]-[7]

ISO 16017 (see Clause 2 and Reference [8]) and ISO 12219 also focus on measuring vapour-phase

organic chemicals in air.

This document can be applied to measure vapour phase organic compounds in indoor environments

that include buildings with varying designs and purposes and cabins for different modes of transport,

as well as measurement in product emission test chambers. These measurements can be for a

range of purposes as described in ISO 16000-1 and ISO 16000-5, therefore the requirement for the

measurement may be well defined by the task descriptor or may be quite open. For example, the task

may be to determine a specific list of target chemicals with a defined sampling time and sensitivity

of measurement or it may be to investigate the cause of a reported and poorly understood indoor air

quality problem. Depending upon the task of measurement the user of this document should select the

most appropriate sampling and analytical instrumentation and conditions. This document provides

that information in the normative part combined with informative guidance. Figure 1 refers to the most

critical parts of the standard with regard to selection of the most appropriate methodology for the task

®1)

to be undertaken. Tenax TA only or multisorbents can be used to capture ranges of vapour phase

organic compounds. Multisorbents are used for wider ranges and may improve recovery of compounds.

Figure 1 — Measurement scheme showing different ways of analysing air samples depending on

the respective task including target compounds

1) Tenax TA is a trade name of a product supplied by Buchem. This information is given for the convenience of

users of this document and does not constitute an endorsement by ISO of the product named. Equivalent products

may be used, if they can be shown to lead to the same results.
© ISO 2021 – All rights reserved v
---------------------- Page: 5 ----------------------
FINAL DRAFT INTERNATIONAL STANDARD ISO/FDIS 16000-6:2021(E)
Indoor air —
Part 6:
Determination of organic compounds (VVOC, VOC, SVOC) in
indoor and test chamber air by active sampling on sorbent
tubes, thermal desorption and gas chromatography using
MS or MS FID
1 Scope

This document specifies a method for determination of volatile organic compounds (VOC) in indoor

air and in air sampled for the determination of the emission from products or materials used in indoor

environments (according to ISO 16000-1) using test chambers and test cells. The method uses sorbent

sampling tubes with subsequent thermal desorption (TD) and gas chromatographic (GC) analysis

employing a capillary column and a mass spectrometric (MS) detector with or without an additional

[13]
flame ionisation detector (FID) .

The method is applicable to the measurement of most GC-compatible vapour-phase organic compounds

at concentrations ranging from micrograms per cubic metre to several milligrams per cubic metre.

Many very volatile organic compounds (VVOC) and semi-volatile organic compounds (SVOC) can be

analysed depending on the sorbents used.
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 16000-1, Indoor air — Part 1: General aspects of sampling strategy

EN 13137, Workplace atmospheres – Pumps for personal sampling of chemical and biological agents –

Requirements and test methods
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

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

— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
3.1
semi-volatile organic compound
SVOC

organic compound eluting after n-hexadecane on a gas chromatographic column specified as a 5 %

phenyl 95 % methyl polysiloxane phase capillary gas chromatographic column

Note 1 to entry: Note to entry: The vapour-fraction of SVOC ranging in volatility to n-C can also be analysed by

thermal desorption GC-MS but requires specific sampling and analytical conditions for optimum performance

[22,25]
© ISO 2021 – All rights reserved 1
---------------------- Page: 6 ----------------------
ISO/FDIS 16000-6:2021(E)
3.2
volatile organic compound
VOC

organic compound eluting between and including n-hexane and n-hexadecane on a gas chromatographic

column specified as a 5 % phenyl 95 % methyl polysiloxane phase capillary gas chromatographic

column
3.3
very volatile organic compound
VVOC

organic compound eluting before n-hexane on a gas chromatographic column specified as 5 % phenyl

95 % methyl polysiloxane phase capillary gas chromatographic column
3.4
total volatile organic compounds
TVOC

sum of the concentration of the identified and unidentified volatile organic compounds (3.2) calculated

as detailed in Annex A
3.5
total semi-volatile organic compounds
TSVOC

sum of the concentrations of identified and unidentified semi-volatile organic compounds (3.1) and

calculated as detailed in Annex A

Note 1 to entry: The limit of volatility of SVOCs included in the TSVOC sum may be defined by the specific task

list.
3.6
target compound

individual vapour phase compound in indoor air with a concentration determined quantitatively and

reported as a result of this method
3.7
task list

specific list of requirements for sampling and analysis defined prior to testing and reflected in the

reporting of the results

Note 1 to entry: The requirements may include a specific target list with or without associated limit criteria, and/

or require investigations of unknowns. They may also include particular control of aspects such as the location,

duration and frequency of sampling.
3.8
laboratory blank

conditioned sorbent tube from the batch selected for each sampling exercise, retained in the laboratory,

sealed with long term storage caps throughout the sampling exercise to be used as a blank tube

Note 1 to entry: These tubes are analysed with the sampled tubes.
3.9
field blank

conditioned sorbent tube from the batch used for the sampling exercise, subjected to the same handling

procedure in the field as the sample tubes, including removal and replacement of storage caps, but not

used for sample collection
3.10
internal standard

compound of known concentration added to a sample to facilitate the qualitative identification and/or

quantitative determination of the sample components
2 © ISO 2021 – All rights reserved
---------------------- Page: 7 ----------------------
ISO/FDIS 16000-6:2021(E)
4 Abbreviated terms
For the purpose of this document, the following abbreviated terms apply:
FID flame ionisation detector
GC gas chromatograph
MS mass spectrometer
SVOC semi-volatile organic compounds
TD thermal desorption
TIC total ion chromatogram
TSVOC total semi-volatile organic compounds
TVOC total volatile organic compounds
VOC volatile organic compounds
VVOC very volatile organic compounds
5 Principle

A measured volume of sample air is actively collected from indoor air, vehicle interior air, an emission

test chamber (see ISO 16000-9, ISO 12219-4, ISO 12219-6) or an emission test cell (see ISO 16000-10) by

drawing through one (or more) sorbent tubes. VOC, VVOC and SVOC are retained by the sorbent tube,

and the compounds are subsequently analysed in the laboratory to determine the identity, retained

mass and associated air concentration of as many individual compounds as required by the specific

test. Depending upon the range of target compounds the most appropriate sorbent tube(s), sampling

and analytical conditions are applied. The collected compounds are desorbed by heat and transferred

under inert carrier gas via a focussing trap into a gas chromatograph equipped with a capillary column

and a mass spectrometer, with or without an additional flame ionisation detector (FID).

6 Reagents and materials
6.1 Organic compounds for calibration of chromatographic quality

6.2 Dilution solvent for preparing calibration blend solution for liquid spiking. Shall be of of

chromatographic quality, free from compounds co-eluting with the compound(s) of interest (6.1)

6.3 Sorbents
6.3.1 General

Multiple sorbents, suitable for thermal desorption, are commercially available. They range in strength

from very retentive sorbents required to retain and release VVOC to very weak sorbents suitable

for quantitative sampling and release of SVOC. For particulate sorbents, the relevant particle size is

0,18 mm to 0,60 mm (80 mesh – 30 mesh). For a detailed list of sorbents see Annex D.

6.3.2 Quartz wool or glass/quartz beads, clean (i.e. do not produce analytically significant artefacts)

and not prone to particle formation.
© ISO 2021 – All rights reserved 3
---------------------- Page: 8 ----------------------
ISO/FDIS 16000-6:2021(E)

6.3.3 Porous Polymers, i.e. Tenax TA particle size approx. 0,25 mm to approx.0,6 mm (60 mesh

® ®

to 30 mesh). Tenax TA is a porous polymer based on 2,6-diphenyleneoxide. Manufactured Tenax TA

contains quantities of impurities, which shall be removed before using it for air sampling.

®2) ®3)

6.3.4 “Carbon black” sorbents, such as Carbopack X or Carbograph 5 TD , particle size 0,25 mm

to 0,5 mm (60 mesh to 40 mesh). Hydrophobic carbon sorbents suitable for VOC and VVOC with vapour

pressures below those typical for C hydrocarbons.

6.3.5 Carbon molecular sieve (very strong) sorbents can also be used at the non-sampling end of

the tube for trapping VVOC with vapour pressures above those typical for C hydrocarbons. However,

note that these sorbents are not completely hydrophobic. Therefore, if such sorbents are included, the

tube needs to be dry purged in the sampling direction before analysis.
6.4 Preparing calibration standards on sorbent tubes

As many identified substances as possible, or as required, should be calibrated using original reference

compounds. Standards should be introduced to the sampling end of conditioned sorbent tubes using

either liquid or gas phase standards.
6.4.1 Gas-phase standards

Standard atmospheres of known concentrations of the compound(s) of interest, shall be prepared by a

[1] [2] 3

recognized procedure such as ISO 6141 or ISO 6145 . Typical concentrations are around 100 µg/m

but levels will vary depending on test requirements. Alternatively, gas standards of appropriate quality

and concentration shall be sourced commercially.

If the concentrations in any prepared standard atmosphere are not traceable to primary standards and/

or if the inertness and stability of the atmospheres generated cannot be guaranteed, the concentration

shall be confirmed using an independent procedure.

NOTE Producing gas phase standards of reactive and/or high boiling compounds can be particularly

difficult. Frequent monitoring of the standard is needed.
6.4.2 Loading sorbent tubes with gas-phase standards

Pass a known volume of standard atmosphere or gas standard through a conditioned sorbent tube from

the sampling end, e.g. by means of a pump operating at 50 ml/min.

The volume of gas-phase standard sampled shall not exceed the breakthrough volume of sorbent tube

for any of the compounds of interest.

After loading disconnect and seal the tube. Prepare fresh standards with each batch of samples. For

indoor air and emission test chamber studies, load sorbent tubes with e.g. 100 ml, 200 ml, 400 ml, 1 l, 2

l, 4 l or 10 l of the 100 µg/m standard atmosphere selected.
6.4.3 Calibration blend solution for liquid spiking

Standard solution concentrations will vary depending on test requirements. The selected compound(s)

shall be prepared or obtained as a liquid standard in chromatographic-grade solvent (e.g. in methanol)

at an appropriate level – typically between 10 ng/µl and 1000 ng/µl – depending on system sensitivity

and the analytical conditions selected, for example split ratios. A suitably precise micro-syringe shall

2) Carbopack X is a trade name of Supelco. This information is given for the convenience of users of this document

and does not constitute an endorsement by ISO of the product named. Equivalent products may be used if they can

be shown to lead to the same results.

3) Carbograph 5 TD is a trade name of Lara. This information is given for the convenience of users of this

document and does not constitute an endorsement by ISO of the product named. Equivalent products may be used,

if they can be shown to lead the the same results.
4 © ISO 2021 – All rights reserved
---------------------- Page: 9 ----------------------
ISO/FDIS 16000-6:2021(E)

be used to introduce 1 µl aliquots of the standard solution onto the sampling end of sorbent tubes in a

stream of inert gas as described in 6.4.4. 1 µl is the suggested volume unless solvent can be selectively

and efficiently purged without jeopardising breakthrough of the most volatile compound(s) of interest.

The stability and safe storage times of calibration blend solutions shall be determined. Fresh standard

solutions shall be prepared accordingly or if there is evidence of deterioration, e.g. reactions between

alcohols and ketones.
6.4.4 Loading sorbent tubes with liquid standards

The sampling end of a sorbent tube is fitted to the unheated injection unit of the gas chromatograph (GC)

(see 7.6) through which inert purge gas is passed at 100 ± 10 ml/min, and a maximum 1 µl aliquot of an

appropriate standard solution is injected through the septum. After 5 min, the tube is disconnected and

sealed. Prepare fresh standard tubes with each batch of samples.

NOTE 1 It is more difficult to selectively purge solvent from multi-sorbent tubes, particularly those containing

strong sorbents. Smaller injection volumes are recommended for stronger sorbents and multi-sorbent tubes.

Introducing liquid standards onto sorbent tubes via a GC injector is considered the optimum approach

to liquid standard introduction, as components reach the sorbent bed in the vapour phase.

Calibration mixtures should be prepared in controlled ambient temperature conditions. Before use,

temper the solutions accordingly.

NOTE 2 When preparing standard tubes from liquid standards containing SVOC analytes, efficient transfer is

enhanced if the configuration of the injector allows the tip of the syringe to make gentle contact with the sorbent

retaining mechanism (e.g. gauze or frit) at the sampling end of the tube.

NOTE 3 It is important to keep liquid standard injection volumes to 1 µl or less unless the solvent can be

selectively purged from the tube prior to analysis. Using small injection volumes minimises the difference

between standards and samples during analysis thus minimising uncertainty.

NOTE 4 Standard tubes containing VVOC are more typically prepared either from standard atmospheres (see

6.4.1 and 6.4.5) or from concentrated gas standards sourced commercially. It is appropriate for concentrated gas

standards to be introduced to the sampling end of sorbent tubes in a stream of carrier gas via an unheated GC

injector or similar device.

An internal standard can be added by mixing with the calibration solution or by spiking separately.

NOTE 5 If standard tubes are being prepared by introducing aliquots from more than one standard solution

or gas, it is appropriate to first introduce the standard containing higher boiling components and to introduce

the most volatile organic compounds last. This minimizes risk of analyte breakthrough during the standard tube

loading process.

The purity of the inert carrier gas used to purge sorbent tubes during standard introduction (e.g. He,

Ar, N2) should permit the detection of an injection of 0,5 ng toluene. The quality of the carrier gas is of

great importance, as any contaminants contained in the gas are enriched on the sorbent together with

the substances to be analysed.

Other techniques such as direct liquid spiking onto the sorbent bed without gas stream applied are

also possible. In this case it is important to use tubes where the syringe needle can directly reach the

sorbent bed.
6.4.5 Commercial, pre-loaded standard tubes

Certified pre-loaded standard tubes are available and can be used for establishing analytical quality

control and for routine calibration.
7 Apparatus
Ordinary laboratory apparatus and in particular the following:
© ISO 2021 – All rights reserved 5
---------------------- Page: 10 ----------------------
ISO/FDIS 16000-6:2021(E)
7.1 Sorbent tubes of stainless steel or glass,
7.1.1 General

Tubes with outside diameter of 6,4 mm (0,25 inch), inside diameter of 5 mm, and of length 89 mm (3,5

inch) fulfil the requirement and are used in many commercial thermal desorbers. Use deactivated glass

wool or other suitable mechanism, e.g. stainless-steel frit, to retain the sorbent in the tube. Conditioned

and sampled sorbent tubes shall be effectively sealed, e.g. with metal screw caps and combined

polytetrafluoroethene (PTFE) ferrules. Alternative tube dimensions may be applied if appropriate

performance data concerning trapping and recovery of target compounds is available as well as

information on safe sampling volume (SSV).

NOTE 1 The unit inch is not allowed in ISO documents; inch equivalents are given for information only.

Pre-packed sorbent tubes are available c
...

SLOVENSKI STANDARD
oSIST ISO/DIS 16000-6:2021
01-februar-2021
Notranji zrak - 6. del: Določevanje hlapnih organskih spojin (VVOC, VOC, SVOC) v
notranjem zraku in zraku v preskusnih komorah z aktivnim vzorčenjem v cevkah z
adsorpcijskim polnilom, termično desorpcijo in plinsko kromatografijo z MS ali
MS-FID

Indoor air - Part 6: Determination of organic compounds (VVOC, VOC, SVOC) in indoor

and test chamber air by active sampling on sorbent tubes, thermal desorption and gas

chromatography using MS or MS FID

Air intérieur - Partie 6: Dosage des composés organiques (COTV, COV, COSV) dans l'air

intérieur et l'air de chambre d'essai par prélèvement actif sur tubes à sorbant, désorption

thermique et chromatographie en phase gazeuse avec détection MS ou MS-FID
Ta slovenski standard je istoveten z: ISO/DIS 16000-6
ICS:
13.040.20 Kakovost okoljskega zraka Ambient atmospheres
oSIST ISO/DIS 16000-6:2021 en,fr

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

---------------------- Page: 1 ----------------------
oSIST ISO/DIS 16000-6:2021
---------------------- Page: 2 ----------------------
oSIST ISO/DIS 16000-6:2021
DRAFT INTERNATIONAL STANDARD
ISO/DIS 16000-6
ISO/TC 146/SC 6 Secretariat: DIN
Voting begins on: Voting terminates on:
2020-07-27 2020-10-19
Indoor air —
Part 6:
Determination of organic compounds (VVOC, VOC, SVOC) in
indoor and test chamber air by active sampling on sorbent
tubes, thermal desorption and gas chromatography using
MS or MS FID
ICS: 13.040.20
THIS DOCUMENT IS A DRAFT CIRCULATED
FOR COMMENT AND APPROVAL. IT IS
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS
BEING ACCEPTABLE FOR INDUSTRIAL,
This document is circulated as received from the committee secretariat.
TECHNOLOGICAL, COMMERCIAL AND
USER PURPOSES, DRAFT INTERNATIONAL
STANDARDS MAY ON OCCASION HAVE TO
BE CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
Reference number
NATIONAL REGULATIONS.
ISO/DIS 16000-6:2020(E)
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 SUPPORTING DOCUMENTATION. ISO 2020
---------------------- Page: 3 ----------------------
oSIST ISO/DIS 16000-6:2021
ISO/DIS 16000-6:2020(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2020

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 2020 – All rights reserved
---------------------- Page: 4 ----------------------
oSIST ISO/DIS 16000-6:2021
ISO/DIS 16000-6:2020(E)
Contents Page

4 Symbols and abbreviated terms ........................................................................................................................................................... 3

8 Conditioning and storage of sorbent tubes ............................................................................................................................... 9

8.2 Strorage of conditioned sorbent tubes before sampling .................................................................................10

9.2 Sampling volumes .............................................................................................................................................................................10

9.3 Storage of loaded samples..........................................................................................................................................................10

9.4 Field blanks for indoor measurements ...........................................................................................................................11

10.1 Determination of VOC, VVOC and SVOC ..........................................................................................................................11

10.1.1 Analytical System .........................................................................................................................................................11

10.1.2 Identification of target compounds ..............................................................................................................13

10.1.3 Quantifiaction of target compounds and compounds according to task list ............13

10.1.4 Determining the quantification limits ........................................................................................................15

10.2 Identified non-target compounds and unidentified compounds .............................................................15

10.3 Other aspects of quality control ............................................................................................................................................16

10.3.1 Laboratory quality checks ....................................................................................................................................16

10.3.2 External references .....................................................................................................................................................16

11 Concentration of analytes in the sampled air ......................................................................................................................16

12 Performance characteristics .................................................................................................................................................................17

Annex A (informative) Total volatile organic compounds (TVOC) and total semi-volatile

organic compounds (TSVOC) ................................................................................................................................................................20

Annex B (informative) Examples of compounds detected in indoor air and from building

products in test chambers .......................................................................................................................................................................21

Annex C (informative) Description of sorbents ......................................................................................................................................27

Annex D (informative) Guide on sorbent usage .....................................................................................................................................28

Annex E (informative) Safe sampling volumes for selected organic vapours .........................................................30

Annex F (informative) Storage recovery of solvents on sorbent tubes ..........................................................................33

© ISO 2020 – All rights reserved iii
---------------------- Page: 5 ----------------------
oSIST ISO/DIS 16000-6:2021
ISO/DIS 16000-6:2020(E)
Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

through ISO technical committees. Each member body interested in a subject for which a technical

committee has been established has the right to be represented on that committee. International

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of

electrotechnical standardization.

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

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

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

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

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

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

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

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

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

constitute an endorsement.

For an explanation on 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 the following

URL: 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 16000-6:2012), which has been

technically revised.
The main changes compared to the previous edition are as follows:
— other sorbents than Tenax TA are allowed to be used;

— descriptions of VVOC and SVOC measurements are included in the mandatory part of the document.

A list of all parts in the ISO 16000 series can be found on the ISO website.
iv © ISO 2020 – All rights reserved
---------------------- Page: 6 ----------------------
oSIST ISO/DIS 16000-6:2021
ISO/DIS 16000-6:2020(E)
Introduction

ISO 16000-1 establishes 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. Aspects of the determination (sampling and analysis) and the sampling strategy

of specific pollutants or groups of pollutants are specified in the subsequent parts of ISO 16000 (see

Foreword).

ISO 16000-5 (dealing with VOC sampling strategy) is a link between ISO 16000-1 (a generic standard

establishing the principles) and this part of ISO 16000, which deals with sampling and analytical

measurements.

ISO 16017 (see Clause 2 and Reference [8]) and ISO 12219 [3]-[7] also focus on measuring vapour-phase

organic chemicals in air.

This standard can be applied to measure vapour phase organic compounds in indoor environments

that include buildings with varying designs and purposes and cabins for differnet modes of transport,

as well as measurement in product emission test chambers. These measurements can be for a range of

purposes as described in ISO 16000-1 and −5, therefore the requirement for the measurement may be

well defined by the task descriptor or may be quite open. For example, the task may be to determine a

specific list of target chemicals with a defined sampling time and sensitivity of measurement or it may

be to investigate the cause of a reported and poorly understood indoor air quality problem. Depending

upon the task of measurement the user of this standard must select the most appropriate sampling and

analytical instrumentation and conditions. This standard provides that information in the normative

part combined with informative guidance. Figure 1 refers to the most critical parts of the standard with

regard to selection of the most appropriate methodology for the task to be undertaken. Tenax TA only

or multisorbents can be used to capture ranges of vapour phase organic compounds. Multisorbents are

used for wider ranges and may improve recovery of compounds.

Figure 1 — Measurement scheme showing different ways of analysing air samples depending on

the respective task including target compounds
© ISO 2020 – All rights reserved v
---------------------- Page: 7 ----------------------
oSIST ISO/DIS 16000-6:2021
---------------------- Page: 8 ----------------------
oSIST ISO/DIS 16000-6:2021
DRAFT INTERNATIONAL STANDARD ISO/DIS 16000-6:2020(E)
Indoor air —
Part 6:
Determination of organic compounds (VVOC, VOC, SVOC) in
indoor and test chamber air by active sampling on sorbent
tubes, thermal desorption and gas chromatography using
MS or MS FID
1 Scope

This part of ISO 16000 specifies a method for determination of volatile organic compounds (VOCs) in

indoor air and in air sampled for the determination of the emission from products or materials used

in indoor environments (according to ISO 16000-1) using test chambers and test cells. The method

uses sorbent sampling tubes with subsequent thermal desorption (TD) and gas chromatographic (GC)

[13]

analysis employing a capillary column and a mass spectrometric (MS) detector with or without

additional Flame Ionisation detector (FID).

The method is applicable to the measurement of most GC-compatible vapor-phase organic compounds

at concentrations ranging from micrograms per cubic metre to several milligrams per cubic metre.

Many very volatile organic compounds (VVOC) and semi-volatile organic compounds (SVOC) can be

analysed depending on sorbents used.
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 16000-1, Indoor air — Part 1: General aspects of sampling strategy

ISO 16017-1:2000, Indoor, ambient and workplace air — Sampling and analysis of volatile organic

compounds by sorbent tube/thermal desorption/capillary gas chromatography — Part 1: Pumped sampling

EN 16516:2017, Construction products: Assessment of release of dangerous substances. Determination of

emissions into indoor air
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

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

— IEC Electropedia: available at http:// www .electropedia .org/
— ISO Online browsing platform: available at https:// www .iso .org/ obp
© ISO 2020 – All rights reserved 1
---------------------- Page: 9 ----------------------
oSIST ISO/DIS 16000-6:2021
ISO/DIS 16000-6:2020(E)
3.1
semi-volatile organic compound
SVOC

Organic compound eluting after n-hexadecane and up to and including n-C on a gas chromatographic

column specified as a 5% phenyl 95% emthyl polysiloxane capillary column.

Note 1 to entry: The vapour-fraction of SVOC ranging in volatility from n-C to n-C can also be analysed by

30 44

thermal desorption GC-MS but requires specific sampling and analytical conditions for optimum performance

[22, 25]
3.2
volatile organic compound
VOC

Organic compound eluting between and including n-hexane and n-hexadecane on a gas chromatographic

column specified as a 5% phenyl 95% methyl polysiloxane capillary column.
3.3
very volatile organic compound
VVOC

Organic compound eluting before n-hexane on a gas chromatographic column specified as 5% phenyl

95% mehtyl polysiloxnae capillary column.
3.4
total volatile organic compounds
TVOC

Sum of the concentration on the identified and unidentified volatile organic compounds, as defind in 3.2

and calculated as detailed in Annex A
3.5
total semi-volatile organic compounds
TSVOC

Sum of the concentrations of identified and unidentified semi-volatile organic compounds as defined in

3.1 and calculated as detailed in Annex A.
3.6
target compound

Individual vapour phase compound in indoor air with a concentration determined quantitatively and

reported as a result of this method
3.7
task list

Specific list of requirements for sampling and analysis defined prior to testing and reflected in the

reporting of the results

Note 1 to entry: The requirements may include a specific target list with or without associated limit criteria, and/

or require investigations of unknowns. They may also include particular control of aspects such as the location,

duration and frequency of sampling.
3.8
laboratory blank

Conditioned sampling tube from the batch selected for each sampling exercise, retained in the

laboratory, sealed with long term storage caps throughout the sampling exercise to be used as a blank

tube. These tubes are analysed with the sampled tubes
3.9
field blank

A conditioned sample tube from the batch used for the sampling exercise, subjected to the same

handling procedure in the field as the sample tubes, including removal and replacement of storage caps,

but not used for sample collection
2 © ISO 2020 – All rights reserved
---------------------- Page: 10 ----------------------
oSIST ISO/DIS 16000-6:2021
ISO/DIS 16000-6:2020(E)
3.10
internal standard

Compound of known concentration added to a sample to facilitate the qualitative identification and/or

quantitative determination of the sample components
4 Symbols and abbreviated terms
For the purpose of this document, the following abbreviated terms apply:
VOC volatile organic compounds
VVOC very volatile organic compound
SVOC semi-volatile organic compounds
TVOC total volatile organic compounds
TSVOC total semi-volatile organic compounds
TIC total ion chromatogram
MS mass spectrometric detector
FID flame ionisation detector
GC gas chromatograph
TD thermal desorption
5 Principle

A measured volume of sample air is actively collected from indoor air, vehicle interior air and an emission

test chamber (see ISO 16000-9, ISO 12219-4, ISO 12219-6) or an emission test cell (see ISO 16000-10)

by drawing through one (or more) sorbent tube. VOC, VVOC and SVOC are retained by the sorbent tube,

and the compounds are subsequently analysed in the laboratory to determine the identity, retained

mass and associated air concentration of as many individual compounds as required by the specific

test. Depending upon the range of target compounds the most appropriate sorbent tube(s), sampling

and analytical conditions are applied. The collected compounds are desorbed by heat and transferred

under inert carrier gas via a focussing trap into a gas chromatograph equipped with a capillary column

and a mass spectrometric detector, with or without an additional flame ionization detector (FID).

6 Reagents and materials
6.1 Organic compounds for calibration of chromatographic quality

6.2 Dilution solvent for preparing calibration blend solution for liquid spiking, of chromatographic

quality, free from compounds co-eluting with the compound(s) of interest (6.1)
6.3 Solid sorbents
6.3.1 Introduction

Multiple sorbents, suitable for thermal desorption, are commercially available. They range in strength

from very retentive sorbents required to retain and release VVOC to very weak sorbents suitable

for quantitative sampling and release of SVOC. For particulate sorbents, the relevant particle size is

0,18 mm to 0,60 mm (30 mesh to 80 mesh). For a detailed list of sorbents see Annex D.

© ISO 2020 – All rights reserved 3
---------------------- Page: 11 ----------------------
oSIST ISO/DIS 16000-6:2021
ISO/DIS 16000-6:2020(E)

6.3.2 Quartz wool or glas/quartz beads, clean (i.e. do not produce analytically significant artefacts)

and not prone to particle formation
®1)

6.3.3 Porous Polymers, i.e. Tenax TA particle size ~0,25 mm to ~0,6 mm (30 mesh to 60 mesh).

® ®

Tenax TA is a porous polymer based on 2,6-diphenyleneoxide. Manufactured Tenax TA contains

quantities of impurities, which shall be removed before using it for air sampling

®2) ®3)

6.3.4 “Carbon black” sorbents, such as Carbopack X or Carbograph 5 TD , particle size 0,25 mm

to 0,5 mm (40 mesh to 60 mesh). Hydrophobic carbon sorbents suitable for VOC and VVOC with vapour

pressures below those typical for C hydrocarbons

6.3.5 Carbon melcular sieve (very strong) sorbents can also be used at the non-sampling end of the

tube for trapping VVOC with vapour pressures above those typical for C hydrocarbons. However, note

that these sorbents are not completely hydrophobic. Therefore, if such sorbents are included, the tube

needs to be dry purged in the sampling direction before analysis
6.4 Preparing calibration standards on sorbent tubes

As many identified substances as possible, or as required, should be calibrated using original reference

compounds. Standards should be introduced to the sampling end of conditioned sorbent tubes using

either liquid or gas phase standards.
6.4.1 Gas-phase standards

Standard atmospheres of known concentrations of the compound(s) of interest, shall be prepared by a

[1] [2] 3

recognized procedure such as ISO 16141 or ISO 6145 . Typical concentrations are around 100 µg/m

but levels will vary depending on test requirements. Alternatively, gas standards of appropriate quality

amd concentration shall be sourced commercially.

If the concentrations in any prepared standard atmosphere are not traceable to primary standards and/

or if the inertness and stability of the atmospheres generated cannot be guaranteed, the concentration

shall be confirmed using an independent procedure.

NOTE Producing gas phase standards of reactive and/or high boiling compounds can be particularly

difficult. Frequent monitoring of the standard will be needed.
6.4.2 Loading sorbent tubes with gas-phase standards

Pass a known volume of standard atmosphere or gas standard through a conditioned sorbent tube from

the sampling end, e.g. by means of a pump operating at 50 ml/min.

The volume of gas-phase standard sampled shall not exceed the breakthrough volume of sorbent tube

for any of the compounds of interest.

After loading disconnect and seal the tube. Prepare fresh standards with each batch of samples. For

indoor air and test chamber air load sorbent tubes with e.g. 100 ml, 200 ml, 400 ml, 1l, 2l, 4l or 10l of the

100 µg/m standard atmosphere selected.

1) Tenax TA is a trade name of a product supplied by Buchem. This information is given for the convenience of

users of this document and does not constitute an endorsement by ISO of the product named. Equivalent products

may be used, if they can be shown to lead to the same results.

2) Carbopack X is a trade name of Supelco. This information is given for the convenience of users of this document

and does not constitute an endorsement by ISO of the product named. Equivalent products may be used if they can

be shown to lead to the same results

3) Carbograph 5 TD is a trade name of Lara. This information is given for the convenience of users of this

document and does not constitute an endorsement by ISO of the product named. Equivalent products may be used,

if they can be shown to lead the the same results.
4 © ISO 2020 – All rights reserved
---------------------- Page: 12 ----------------------
oSIST ISO/DIS 16000-6:2021
ISO/DIS 16000-6:2020(E)
6.4.3 Calibration blend solution for liquid spiking

Standard solution concentrations will vary depending on test requirements. The selected compound(s)

shall be prepared or obtained as a liquid standard in chromatographic-grade solvent (e.g. in methanol)

at an appropriate level – typically between 10 ng/mµl and 1000ng/µl – depending on system sensitivity

and the analytical conditions selected, for example split ratios. A suitably precise micro-syringe shall be

used to introduce 1 µl aliquots of the check material onto the sampling end of sorbent tubes in a stream

of inert gas as described. 1 µl is the suggested volume unless solvent can be selectively and efficiently

purged without jeopardising breakthrough of the most volatile compounds(s) of interest.

The stability and safe storage times of calibration blend solutions shall be determined. Fresh standard

solutions shall be prepared accordingly or if there is evidence of deterioration, e.g. reactions between

alcohols and ketones.

Other techniques such as direct liquid spiking onto the sorbent bed without gas stream applied are

also possible. In this case it is important to use tubes where the syringe needle can directly reach the

sorbent bed.
6.4.4 Loading sorbent tubes with liquid standards

The sampling end of of a sorbent tube is fitted to the unheated injection unit of the gas chromatograph

(GC) (7.6) through which inert purge gas is passed at 100 ml/min, and a maximum 1µl aliquot of an

appropriate standard solution is injected through the septum. After 5 min, the tube is disconnected and

sealed. Prepare fresh standard tubes with each batch of samples.

NOTE 1 Multi-sorbent tubes, in particular with stronger sorbents are more difficult to solvent and standard

solution. Smaller injection volumes are recommended for stronger sorbents and multi-sorbent tubes.

Introducing liquid standards on to sorbent tubes via a GC injector is considered the optimum approach

to liquid standard introduction, as components reach the sorbent bed in the vapour phase.

Calibration mixtures should be prepared in controlled ambient temperature conditions. Before use,

temper the solutions accordingly.

NOTE 2 When preparing standard tubes from liquid standards containing SVOC analytes, efficient transfer is

enhanced if the configuration of the injector allows the tip of the syringe to make gentle contact with the sorbent

retaining mechanism (e.g. gauze or frit) at the sampling end of the tube. It is important to keep liquid standard

injection volumes to 1 µl or less unless the solvent can be selectively purged from the tube prior to analysis.

Using small injection volumes minimises the difference between standards and samples during analysis thus

minimising uncertainty.

NOTE 3 Standard tubes containing VVOC are more typically prepared either from standard atmospheres (see.

6.4 and 6.5) or from concentrated gas standards sourced commercially. It is appropriate for concentrated gas

standards to be introduced to the sampling end of sorbent tubes in a stream of carrier gas via an unheated GC

injector or similar device.

An internal standard can be added by mixing with the calibration solution or by spiking separately.

NOTE 4 If standard tubes are being prepared by introducing aliquots from more than one standard

...

PROJET
NORME ISO/FDIS
FINAL
INTERNATIONALE 16000-6
ISO/TC 146/SC 6
Air intérieur —
Secrétariat: DIN
Début de vote:
Partie 6:
2021-05-05
Dosage des composés organiques
Vote clos le:
(COTV, COV, COSV) dans l'air
2021-06-30
intérieur et l'air de chambre d'essai
par prélèvement actif sur tubes à
sorbant, désorption thermique et
chromatographie en phase gazeuse
avec détection MS ou MS-FID
Indoor air —
Part 6: Determination of organic compounds (VVOC, VOC, SVOC) in
indoor and test chamber air by active sampling on sorbent tubes,
thermal desorption and gas chromatography using MS or MS FID
LES DESTINATAIRES DU PRÉSENT PROJET SONT
INVITÉS À PRÉSENTER, AVEC LEURS OBSER-
VATIONS, NOTIFICATION DES DROITS DE PRO-
PRIÉTÉ DONT ILS AURAIENT ÉVENTUELLEMENT
CONNAISSANCE ET À FOURNIR UNE DOCUMEN-
TATION EXPLICATIVE.
OUTRE LE FAIT D’ÊTRE EXAMINÉS POUR
ÉTABLIR S’ILS SONT ACCEPTABLES À DES FINS
INDUSTRIELLES, TECHNOLOGIQUES ET COM-
Numéro de référence
MERCIALES, AINSI QUE DU POINT DE VUE
ISO/FDIS 16000-6:2021(F)
DES UTILISATEURS, LES PROJETS DE NORMES
INTERNATIONALES DOIVENT PARFOIS ÊTRE
CONSIDÉRÉS DU POINT DE VUE DE LEUR POSSI-
BILITÉ DE DEVENIR DES NORMES POUVANT
SERVIR DE RÉFÉRENCE DANS LA RÉGLEMENTA-
TION NATIONALE. ISO 2021
---------------------- Page: 1 ----------------------
ISO/FDIS 16000-6:2021(F)
DOCUMENT PROTÉGÉ PAR COPYRIGHT
© ISO 2021

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

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

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

ISO copyright office
Case postale 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Genève
Tél.: +41 22 749 01 11
E-mail: copyright@iso.org
Web: www.iso.org
Publié en Suisse
ii © ISO 2021 – Tous droits réservés
---------------------- Page: 2 ----------------------
ISO/FDIS 16000-6:2021(F)
Sommaire Page

Avant-propos ..............................................................................................................................................................................................................................iv

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

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

3 Termes et définitions ....................................................................................................................................................................................... 1

4 Abréviations .............................................................................................................................................................................................................. 3

5 Principe .......................................................................................................................................................................................................................... 3

6 Réactifs et matériaux ....................................................................................................................................................................................... 3

7 Appareillage .............................................................................................................................................................................................................. 6

8 Conditionnement et conservation des tubes à sorbant ............................................................................................11

8.1 Conditionnement ...............................................................................................................................................................................11

8.2 Conservation des tubes à sorbant conditionnés avant prélèvement ....................................................11

9 Prélèvement ...........................................................................................................................................................................................................11

9.1 Prélèvement d’air ...............................................................................................................................................................................11

9.2 Volumes de prélèvement .............................................................................................................................................................12

9.3 Conservation des échantillons chargés ...........................................................................................................................12

9.4 Blancs de site .........................................................................................................................................................................................12

10 Analyse .........................................................................................................................................................................................................................13

10.1 Dosage des COV, des COTV et des COSV..........................................................................................................................13

10.1.1 Système analytique .....................................................................................................................................................13

10.1.2 Identification des composés cibles ...............................................................................................................15

10.1.3 Quantification des composés cibles et des composés en fonction de la liste

de tâches ..............................................................................................................................................................................15

10.1.4 Détermination de la limite inférieure de quantification .................. ...........................................18

10.2 Composés non cibles identifiés et composés non identifiés ........................................................................18

11 Concentration en analytes de l’air prélevé .............................................................................................................................18

12 Caractéristiques de performance ....................................................................................................................................................20

13 Rapport d’essai ....................................................................................................................................................................................................21

14 Contrôle qualité ..................................................................................................................................................................................................21

Annexe A (informative) Composés organiques volatils totaux (COVT) et composés

organiques semi-volatils totaux (COSVT) ................................................................................................................................23

Annexe B (informative) Exemples de composés détectés dans l’air intérieur et émanant des

produits de construction dans les chambres d’essai ...................................................................................................25

Annexe C (informative) Description des sorbants ...............................................................................................................................30

Annexe D (informative) Guide d’utilisation des sorbants ...........................................................................................................31

Annexe E (informative) Volumes limites de prélèvement des vapeurs organiques sélectionnées ..33

Annexe F (informative) Taux de récupération des composés fixés sur des tubes à sorbant

après conservation ..........................................................................................................................................................................................36

Bibliographie ...........................................................................................................................................................................................................................38

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

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

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

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

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

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

concerne la normalisation électrotechnique.

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

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

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

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

.iso .org/ directives).

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

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

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

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

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

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

Les appellations commerciales éventuellement mentionnées dans le présent document sont données

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

engagement.

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

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

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

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

Le présent document a été élaboré par le comité technique ISO/TC 146, Qualité de l’air, sous-comité SC 6,

Air intérieur.

Cette troisième édition annule et remplace la deuxième édition (ISO 16000-6:2012), qui a fait l’objet

d’une révision technique. Les principales modifications par rapport à l’édition précédente sont les

suivantes:
— l’utilisation d’autres sorbants que le Tenax TA est autorisée;

— les descriptions des mesurages des COTV et COSV sont incluses dans la partie obligatoire du présent

document.

Une liste de toutes les parties de la série ISO 16000 se trouve sur le site web de l’ISO.

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

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

L’ISO 16000-1 établit les exigences générales relatives au mesurage des polluants de l’air intérieur et les

conditions qu’il est important de respecter avant ou pendant l’échantillonnage de polluants isolés ou de

groupes de polluants. Les détails relatifs au dosage (échantillonnage et analyse) ainsi que la stratégie

d’échantillonnage des polluants ou des groupes spécifiques de polluants sont spécifiés dans les autres

parties de l’ISO 16000 (voir l’Avant-propos).

L’ISO 16000-5 (traitant de la stratégie d’échantillonnage des COV) est un lien entre l’ISO 16000-1 (une

norme générique établissant les principes) et la présente partie de l’ISO 16000 traitant du prélèvement

et des mesurages analytiques.
[3]-[7]

L’ISO 16017 (voir Article 2 et Référence [8]) et l’ISO 12219 portent également sur les mesurages

des substances chimiques organiques en phase vapeur dans l’air.

Le présent document peut être appliqué pour mesurer les composés organiques en phase vapeur dans

les environnements intérieurs qui comprennent les bâtiments ayant diverses conceptions et fonctions

et les habitacles de différents modes de transport, tout comme pour effectuer des mesurages dans

les chambres d’essai d’émission de produit. Ces mesurages peuvent convenir pour divers objectifs

tels que décrits dans l’ISO 16000-1 et l’ISO 16000-5. Par conséquent, l’exigence relative au mesurage

peut être bien définie par le descripteur de tâche ou peut être relativement ouverte. Par exemple, la

tâche peut consister à déterminer une liste spécifique de substances chimiques cibles avec une durée

de prélèvement et une sensibilité de mesurage définies, ou elle peut consister à étudier la cause d’un

problème de qualité de l’air intérieur qui a été rapporté et mal compris. Selon la tâche du mesurage,

l’utilisateur du présent document doit choisir l’instrumentation et les conditions de prélèvement et

d’analyse les plus appropriées. Le présent document fournit ces informations dans la partie normative,

en association avec des recommandations informatives. La Figure 1 se rapporte aux principales parties

de la norme concernant le choix de la méthode la mieux adaptée à la tâche à entreprendre. Le Tenax

®1)

TA seul ou plusieurs sorbants peuvent être utilisés pour capter divers composés organiques en

phase vapeur. Plusieurs sorbants sont utilisés pour des gammes plus larges et peuvent améliorer la

récupération des composés.

Figure 1 — Schéma de mesurage illustrant différentes façons d’analyser des échantillons d’air

en fonction de la tâche correspondante, y compris des composés cibles

1) Tenax TA est une appellation commerciale d'un produit fourni par Buchem. Cette information est donnée par

souci de commodité à l'intention des utilisateurs du présent document et ne saurait constituer un engagement de

l'ISO à l’égard de ce produit. Des produits équivalents peuvent être utilisés s’il est démontré qu’ils conduisent aux

mêmes résultats.
© ISO 2021 – Tous droits réservés v
---------------------- Page: 5 ----------------------
PROJET FINAL DE NORME INTERNATIONALE ISO/FDIS 16000-6:2021(F)
Air intérieur —
Partie 6:
Dosage des composés organiques (COTV, COV, COSV) dans
l'air intérieur et l'air de chambre d'essai par prélèvement
actif sur tubes à sorbant, désorption thermique et
chromatographie en phase gazeuse avec détection MS ou
MS-FID
1 Domaine d’application

Le présent document spécifie une méthode permettant de doser les composés organiques volatils

(COV) dans l’air intérieur et dans l’air prélevé afin de déterminer l’émission de produits ou de matériaux

utilisés dans les environnements intérieurs (conformément à l’ISO 16000-1) à l’aide de chambres

d’essai et de cellules d’essai. La méthode utilise un prélèvement sur tubes à sorbant puis une désorption

thermique (TD) et une analyse par chromatographie en phase gazeuse (GC) utilisant une colonne

capillaire et un détecteur à spectrométrie de masse (MS) avec ou sans détecteur à ionisation de flamme

[13]
(FID) supplémentaire .

La méthode est applicable au mesurage de la plupart des composés organiques volatils en phase vapeur

avec une analyse GC, à des concentrations allant de quelques microgrammes par mètre cube à plusieurs

milligrammes par mètre cube. De nombreux composés organiques très volatils (COTV) et composés

organiques semi-volatils (COSV) peuvent être analysés en fonction des sorbants utilisés.

2 Références normatives

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

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

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

éventuels amendements).

ISO 16000-1, Air intérieur — Partie 1: Aspects généraux de la stratégie d'échantillonnage

EN 13137, Air des lieux de travail — Pompes pour l’échantillonnage individuel des agents chimiques et

biologiques — Exigences et méthodes d’essai
3 Termes et définitions

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

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

normalisation, consultables aux adresses suivantes:

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

— IEC Electropedia: disponible à l’adresse httpss:// www .electropedia .org/
© ISO 2021 – Tous droits réservés 1
---------------------- Page: 6 ----------------------
ISO/FDIS 16000-6:2021(F)
3.1
composé organique semi-volatil
COSV

composé organique éluant après le n-hexadécane sur une colonne de chromatographie en phase gazeuse

spécifiée comme étant une colonne capillaire de chromatographie en phase gazeuse 5 % phényle et

95 % méthylpolysiloxane

Note 1 à l'article: La fraction vapeur du COSV ayant une volatilité allant jusqu’au n-C44 peut également être

analysée par désorption thermique GC-MS mais requiert des conditions de prélèvement et d’analyse spécifiques

pour obtenir des performances optimales [22,25].
3.2
composé organique volatil
COV

composé organique éluant entre le n-hexane inclus et le n-hexadécane sur une colonne de

chromatographie en phase gazeuse spécifiée comme étant une colonne capillaire de chromatographie

en phase gazeuse 5 % phényle et 95 % méthylpolysiloxane
3.3
composé organique très volatil
COTV

composé organique éluant avant le n-hexane sur une colonne de chromatographie en phase gazeuse

spécifiée comme étant une colonne capillaire de chromatographie en phase gazeuse 5 % phényle et

95 % méthylpolysiloxane
3.4
composés organiques volatils totaux
COVT

somme des concentrations des composés organiques volatils identifiés et non identifiés (3.2), calculée

comme indiqué à l’Annexe A
3.5
composés organiques semi-volatils totaux
COSVT

somme des concentrations des composés organiques semi-volatils identifiés et non identifiés (3.1),

calculée comme indiqué à l’Annexe A.

Note 1 à l'article: La limite de volatilité des COSV inclus dans la somme des COSVT peut être définie par la liste de

tâches spécifique.
3.6
composé cible

composé individuel en phase vapeur présent dans l’air intérieur à une concentration déterminée

quantitativement et rapportée après application de cette méthode
3.7
liste de tâches

liste spécifique des exigences de prélèvement et d’analyse définies avant les essais et mentionnées dans

le compte-rendu des résultats

Note 1 à l'article: Les exigences peuvent comprendre une liste cible spécifique avec ou sans critères limites

associés, et/ou nécessiter l’étude d’inconnues. Elles peuvent également comprendre le contrôle d’éléments tels

que l’emplacement, la durée et la fréquence de prélèvement.
3.8
blanc de laboratoire

tube à sorbant conditionné extrait du lot choisi pour chaque prélèvement, conservé au laboratoire,

fermé à l’aide de bouchons longue conservation tout au long du prélèvement, servant de tube blanc

Note 1 à l'article: à l’Article Ces tubes sont analysés avec les tubes prélevés.
2 © ISO 2021 – Tous droits réservés
---------------------- Page: 7 ----------------------
ISO/FDIS 16000-6:2021(F)
3.9
blanc de site

tube à sorbant conditionné extrait du lot utilisé pour le prélèvement, soumis au même mode opératoire

de manipulation sur site que les tubes d’échantillons, y compris le retrait et le remplacement des

bouchons de conservation, mais non utilisé pour la collecte d’échantillons
3.10
étalon interne

composé de concentration connue, ajouté à un échantillon pour faciliter l’identification qualitative et/

ou la détermination quantitative des composants de l’échantillon
4 Abréviations
Pour les besoins du présent document, les abréviations suivantes s’appliquent:
FID détecteur à ionisation de flamme
GC chromatographe en phase gazeuse
MS spectromètre de masse
COSV composés organiques semi-volatils
TD désorption thermique
TIC chromatogramme d'ions totaux
COSVT composés organiques semi-volatils totaux
COVT composés organiques volatils totaux
COV composés organiques volatils
COTV composés organiques très volatils
5 Principe

Un échantillon d’air est activement prélevé à l’intérieur d’un bâtiment, d’un véhicule, d’une chambre

d’essai d’émission (voir l’ISO 16000-9, l’ISO 12219-4, l’ISO 12219-6) ou d’une cellule d’essai d’émission

(voir l’ISO 16000-10) en aspirant à travers un ou plusieurs tubes à sorbant un volume d’air mesuré. Les

COV, COTV et COSV sont retenus sur le tube à sorbant. Les composés sont ensuite analysés en laboratoire

afin de les identifier, de les quantifier en masse de composé retenue et de déterminer la concentration

dans l’air associée et ce, pour chaque composé individuel exigé par l’essai spécifique. Selon la gamme de

composés cibles, le ou les tubes à sorbant ainsi que les conditions de prélèvement et d’analyse les plus

appropriés sont choisis et appliqués. Les composés recueillis sont désorbés par la chaleur et transportés

par le gaz vecteur inerte via un piège de focalisation puis envoyés vers un chromatographe en phase

gazeuse équipé d’une colonne capillaire et d’un spectromètre de masse, potentiellement complété par

un détecteur à ionisation de flamme (FID).
6 Réactifs et matériaux
6.1 Composés organiques volatils pour étalonnage, de qualité chromatographique.

6.2 Solvant de dilution pour préparer la solution de mélange d’étalonnage pour dopage de liquide.

Doit être de qualité chromatographique, exempt de composés co-éluant avec le ou les composés analysés

Plusieurs sorbants appropriés pour la désorption thermique sont disponibles dans le commerce.

Leur pouvoir sorbant peut aller de très élevé (pour retenir et émettre des COTV) à très faible (pour

le prélèvement quantitatif et l’émission de COSV). Pour les sorbants particulaires, la granulométrie

appropriée est comprise entre 0,18 mm et 0,60 mm (30 mesh à 80 mesh). Pour une liste détaillée des

sorbants, voir l’Annexe D.

6.3.2 Laine de quartz ou billes de verre/quartz, propre(s) (c’est-à-dire, ne produisant pas d’artefacts

ayant une influence sur l’analyse) et non encline(s) à la formation de particules.

6.3.3 Polymères poreux, c’est-à-dire Tenax TA granulométrie d’environ 0,25 mm à environ 0,6 mm

(30 mesh à 60 mesh). Le Tenax TA est un polymère poreux à base d’oxyde de 2,6-diphénylène. Le Tenax

TA fabriqué contient de nombreuses impuretés qui doivent être éliminées avant son utilisation à des

fins de prélèvement de l’air.
®2) ®3)

6.3.4 Sorbants de type noir de carbone, tels que Carbopack X ou Carbograph 5 TD ,

granulométrie 0,25 mm à 0,5 mm (40 mesh à 60 mesh). Sorbants de type carbone hydrophobe, appropriés

aux COV et COTV et ayant des tensions de vapeur inférieures à celles typiques des hydrocarbures en C .

6.3.5 Sorbants (très forts) de type tamis moléculaire carboné, également utilisables au niveau de

l’extrémité du tube ne servant pas au prélèvement pour piéger les COTV dont les tensions de vapeur

sont supérieures à celles typiques des hydrocarbures en C . Noter toutefois que ces sorbants ne sont pas

totalement hydrophobes. Par conséquent, si ces sorbants sont inclus, il faut purger le tube à sec dans la

direction de prélèvement avant l’analyse.
6.4 Préparation des étalons sur des tubes à sorbant

Il convient d’étalonner le plus possible de substances identifiées, ou autant que nécessaire, en utilisant

les composés de référence standards. Il convient d’introduire des étalons en phase liquide ou gazeuse

dans l’extrémité de prélèvement des tubes à sorbant conditionnés.
6.4.1 Étalons en phase gazeuse

Des atmosphères étalons contenant des concentrations connues en composé(s) analysé(s) doivent être

[1] [2]

préparées en appliquant un mode opératoire homologué tel qu’indiqué dans l’ISO 6141 ou l’ISO 6145 .

Les concentrations types sont d’environ 100 µg/m mais les niveaux peuvent varier en fonction des

exigences d’essai. En variante, des étalons en phase gazeuse de qualité et de concentration appropriées

doivent être achetés dans le commerce.

Si les concentrations dans une atmosphère étalon préparée ne sont pas raccordables à des étalons

primaires et/ou si l’inertie et la stabilité des atmosphères générées ne peuvent pas être garanties, la

concentration doit être confirmée en appliquant un mode opératoire indépendant.

NOTE Il peut être particulièrement difficile de produire des étalons en phase gazeuse de composés réactifs

et/ou à haut point d’ébullition. Il est nécessaire de contrôler régulièrement l’étalon.

2) Carbopack X est une appellation commerciale de Supelco. Cette information est donnée par souci de commodité

à l'intention des utilisateurs du présent document et ne saurait constituer un engagement de l'ISO à l’égard de ce

produit. Des produits équivalents peuvent être utilisés s’il est démontré qu’ils conduisent aux mêmes résultats.

3) Carbograph 5 TD est une appellation commerciale de Lara. Cette information est donnée par souci de

commodité à l'intention des utilisateurs du présent document et ne saurait constituer un engagement de l'ISO à

l’égard de ce produit. Des produits équivalents peuvent être utilisés s’il est démontré qu’ils conduisent aux mêmes

Transférer un volume connu d’atmosphère étalon ou d’étalon en phase gazeuse dans un tube à sorbant

conditionné depuis l’extrémité de prélèvement, par exemple à l’aide d’une pompe fonctionnant à 50 ml/

min.

Le volume d’étalon en phase gazeuse prélevé ne doit pas dépasser le volume de perçage du tube à

sorbant pour aucun des composés analysés.

Après le chargement, détacher le tube, puis le refermer hermétiquement. Préparer de nouveaux tubes

étalons à chaque lot d’échantillons. Dans le cadre des études avec de l’air intérieur et de l’air de chambre

d’essai d’émission, charger les tubes à sorbant avec, par exemple 100 ml, 200 ml, 400 ml, 1 l, 2 l, 4 l ou

10 l de l’atmosphère étalon sélectionnée à 100 µg/m .
6.4.3 Solutions de mélange d’étalonnage pour dopage de liquide

Les concentrations en solution d’étalonnage varient en fonction des exigences d’essai. Le ou les composés

sélectionnés doivent être préparés ou obtenus sous la forme d’un étalon liquide dans un solvant de

qualité chromatographique (par exemple dans du méthanol) à un niveau approprié (généralement entre

10 ng/µl et 1 000 ng/µl) selon la sensibilité du système et les conditions analytiques sélectionnées, par

exemple les rapports de division. Une microseringue de précision doit être utilisée pour introduire des

aliquotes de 1 µl de solution étalon dans l’extrémité de prélèvement des tubes à sorbant dans un flux de

gaz inerte tel que décrit en 6.4.4. Un volume de 1 µl est suggéré, sauf si le solvant peut être sélectivement

et efficacement purgé sans compromettre le perçage du ou des composés analysés les plus volatils.

La stabilité et les durées de conservation sans détérioration des solutions de mélange d’étalonnage

doivent être déterminées. De nouvelles solutions étalons doivent être préparées en fonction du mode

opératoire ou dans le cas de dégradations, dues par exemple à des réactions entre alcools et cétones.

6.4.4 Chargement des étalons en phase liquide dans les tubes à sorbant

L’extrémité de prélèvement d’un tube à sorbant est ajustée sur le dispositif d’injection du chromatographe

en phase gazeuse (GC) (voir 7.6) balayé par du gaz de purge inerte à un débit de 100 ml/min ± 10 ml/min,

et une aliquote de 1 µl maximum d’une solution étalon appropriée est injectée au travers du septum. Au

bout de 5 min, le tube est détaché, puis refermé hermétiquement. Préparer de nouveaux tubes étalons à

chaque lot d’échantillons.

NOTE 1 Il est plus difficile de purger sélectivement le solvant pour des tubes contenant plusieurs sorbants, en

particulier pour ceux contenant des sorbants forts. De plus petits volumes d’injection sont recommandés pour les

tubes contenant des sorbants plus forts et plusieurs sorbants.

L’introduction d’étalons en phase liquide dans des tubes à sorbant à l’aide d’un injecteur de

chromatographe en phase gazeuse est considérée comme constituant l’app
...

ISO/FDIS 16000-6

Indoor air

Indoor air

Air intérieur

Notranji zrak - 6. del: Določevanje hlapnih organskih spojin (VVOC, VOC, SVOC) v notranjem zraku in zraku v preskusnih komorah z aktivnim vzorčenjem v cevkah z adsorpcijskim polnilom, termično desorpcijo in plinsko kromatografijo z MS ali MS-FID

General Information

RELATIONS

Buy Standard

Standards Content (sample)

Questions, Comments and Discussion

Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.

Indoor air

Air intérieur

Notranji zrak - 6. del: Določevanje hlapnih organskih spojin (VVOC, VOC, SVOC) v notranjem zraku in zraku v preskusnih komorah z aktivnim vzorčenjem v cevkah z adsorpcijskim polnilom, termično desorpcijo in plinsko kromatografijo z MS ali MS-FID

General Information

RELATIONS

Buy Standard

Standards Content (sample)

Questions, Comments and Discussion

Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.

This May Also Interest You