Indoor air - Part 33: Determination of phthalates with gas chromatography/mass spectrometry (GC/MS)

This document specifies the sampling and analysis of phthalates in indoor air and describes the
sampling and analysis of phthalates in house dust and in solvent wipe samples of surfaces by means of
gas chromatography/mass spectrometry.
Two alternative sampling and processing methods, whose comparability has been proven in a round
robin test, are specified for indoor air[4]. Sampling can take place using sorbent tubes with subsequent
thermal desorption and GC-MS analysis. Alternatively, sampling can take on other types of sorbent
tubes that are subsequently analysed by solvent extraction with GC-MS.
Depending on the sampling method, the compounds dimethyl phthalate to diisoundecylphthalate
can be analysed in house dust as described in Annex C[8]. The investigation of house dust samples is
only appropriate as a screening method. This investigation only results in indicative values and is not
acceptable for a final assessment of a potential need for action.
Dimethyl phthalate to diisoundecylphthalate can be analysed in solvent wipe samples as described in
Annex B. Solvent wipe samples are suitable for non-quantitative source identification.
NOTE In principle, the method is also suitable for the analysis of other phthalates, adipates and cyclohexane
dicarboxylic acid esters, but this is confirmed by determination of the performance characteristics in each case.
General information on phthalates are given in Annex A.

Air intérieur - Partie 33: Détermination des phthalates par chromatographie en phase gazeuse/spectrométrie de masse (CPG/SM)

ISO 16000-33:2017 sp�cifie le pr�l�vement et l'analyse des phtalates dans l'air int�rieur et d�crit le pr�l�vement et l'analyse des phtalates dans des �chantillons de poussi�res domestiques et des pr�l�vements de surface (frottis) par chromatographie en phase gazeuse/spectrom�trie de masse.
Deux m�thodes possibles de pr�l�vement et de traitement, dont la comparabilit� a �t� d�montr�e au cours d'un essai interlaboratoires, sont sp�cifi�es pour l'air int�rieur[4]. Le pr�l�vement peut �tre r�alis� � l'aide de tubes � sorbant suivi d'une d�sorption thermique et d'une analyse par CPG/SM. En variante, le pr�l�vement peut �tre r�alis� sur d'autres types de tubes � sorbant qui sont ensuite analys�s par extraction au solvant avec analyse par CPG/SM.
Selon la m�thode de pr�l�vement, les compos�s phtalate de dim�thyle � phtalate de diisound�cyle peuvent �tre analys�s dans les poussi�res domestiques, comme d�crit dans l'Annexe C[8]. L'�tude d'�chantillons de poussi�res domestiques est appropri�e uniquement comme m�thode de diagnostic rapide. Cette �tude donne seulement des valeurs indicatives et n'est pas acceptable pour une �valuation finale de la n�cessit� �ventuelle d'une action.
Les compos�s phtalate de dim�thyle � phtalate de diisound�cyle peuvent �tre analys�s dans des frottis comme d�crit dans l'Annexe B. Les frottis conviennent pour l'identification non quantitative des sources.
NOTE En principe, la m�thode convient �galement pour l'analyse d'autres phtalates, adipates et esters d'acide cyclohexane dicarboxylique, mais cela est confirm� dans chaque cas par la d�termination des performances analytiques.
Des informations g�n�rales sur les phtalates sont donn�es dans l'Annexe A.

Notranji zrak - 33. del: Določevanje ftalatov s plinsko kromatografijo/masno spektrometrijo (GC/MS)

Ta dokument določa vzorčenje in analizo ftalatov v notranjem zraku ter opisuje
vzorčenje in analizo ftalatov v hišnem prahu in v vzorcih brisov s topili na površinah s
plinsko kromatografijo/masno spektrometrijo.
Dve alternativni metodi vzorčenja in obdelave, pri čemer je bila njuna primerljivost dokazana z medlaboratorijskimi
preskusi, sta določeni za notranji zrak [4]. Vzorčenje lahko poteka z uporabo cevi s sorbentom ter naknadno
toplotno desorpcijo in analizo s plinsko kromatografijo/masno spektrometrijo (GC-MS). Namesto tega se lahko za vzorčenje uporabijo druge vrste cevi
s sorbentom, ki se naknadno analizirajo pri ekstrakciji s topilom med plinsko kromatografijo/masno spektrometrijo (GC-MS).
Glede na metodo vzorčenja je mogoče spojine od dimetil ftalat do di-izodecil ftalat
analizirati v hišnem prahu, kot je opisano v dodatku C[8]. Preiskava vzorcev hišnega prahu je
primerna le kot metoda preverjanja. Rezultati preiskave so zgolj indikativne vrednosti in niso
sprejemljivi za končno oceno potrebe po morebitnem ukrepanju.
Spojine od dimetil ftalat do di-izodecil ftalat je mogoče analizirati v vzorcih brisov s topilom, kot je opisano
v dodatku B. Vzorci brisov s topili so primerni za nekvantitativno identifikacijo vira.
OPOMBA: Načeloma je metoda primerna tudi za analizo drugih ftalatov, adipatov in estrov cikloheksana
in dikarboksilne kisline, vendar je to v vsakem primeru potrjeno z ugotavljanjem zmogljivostnih lastnosti.
Splošne informacije o ftalatih so navedene v dodatku A.

General Information

Status
Published
Public Enquiry End Date
09-Oct-2018
Publication Date
16-Jun-2019
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
12-Jun-2019
Due Date
17-Aug-2019
Completion Date
17-Jun-2019

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INTERNATIONAL ISO
STANDARD 16000-33
First edition
2017-08
Indoor air —
Part 33:
Determination of phthalates with gas
chromatography/mass spectrometry
(GC/MS)
Air intérieur —
Partie 33: Détermination des phthalates par chromatographie en
phase gazeuse/spectrométrie de masse (CPG/SM)
Reference number
ISO 16000-33:2017(E)
ISO 2017
---------------------- Page: 1 ----------------------
ISO 16000-33:2017(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2017, Published in Switzerland

All rights reserved. Unless otherwise specified, 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
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. +41 22 749 01 11
Fax +41 22 749 09 47
copyright@iso.org
www.iso.org
ii © ISO 2017 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 16000-33:2017(E)
Contents Page

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

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

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

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

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

4 Sampling methods and analytical apparatus .......................................................................................................................... 2

4.1 General ........................................................................................................................................................................................................... 2

4.2 Sampling by adsorption with subsequent thermal desorption .................................................................... 2

4.2.1 Apparatus, operating materials and chemicals ..................................................................................... 2

4.2.2 Preparation of the thermal desorption tube ............................................................................................ 3

4.2.3 Sampling.................................................................................................................................................................................. 3

4.3 Sampling by adsorption and subsequent solvent extraction .......................................................................... 4

4.3.1 Apparatus, operating materials and chemicals ..................................................................................... 4

4.3.2 Preparation of Florisil® and the adsorption tubes ....................................................................... 5

2) 6

4.3.3 Hints to the application of Florisil® ............................................................................................................

4.3.4 Sampling.................................................................................................................................................................................. 6

4.3.5 Sample conditioning ..................................................................................................................................................... 7

5 Calibration .................................................................................................................................................................................................................. 7

5.1 General ........................................................................................................................................................................................................... 7

5.2 Calibration of the thermal desorption method ........................................................................................................... 8

5.3 Calibration of the solvent extraction method ............................................................................................................... 8

6 Identification and quantification ........................................................................................................................................................ 8

6.1 Mass spectrometric analysis ....................................................................................................................................................... 8

7 Establishment of calibration curves and calculation of the analyte mass .............................................14

7.1 Establishment of calibration curves ..................................................................................................................................14

7.2 Calculation of the analyte mass .............................................................................................................................................14

8 Calculation of indoor air concentrations .................................................................................................................................15

9 Performance characteristics .................................................................................................................................................................16

9.1 Detection limit ......................................................................................................................................................................................16

9.2 Quantification limit and problems related to the blank values ..................................................................16

9.3 Reproducibility standard deviation and repeatability standard deviation .....................................17

10 Quality assurance .............................................................................................................................................................................................19

10.1 Method verification and determination of blanks .................................................................................................19

10.1.1 Field blank value of the indoor air.................................................................................................................19

10.1.2 Analytical laboratory blank value ..................................................................................................................19

10.2 Measures for blank value minimization .........................................................................................................................19

10.3 Documents ...............................................................................................................................................................................................20

11 Interferences .........................................................................................................................................................................................................20

Annex A (informative) General information on phthalates .......................................................................................................21

Annex B (informative) Screening phthalates in solvent wipe tests ...................................................................................24

Annex C (informative) Screening phthalates in house dust .......................................................................................................27

Annex D (informative) Practical example for the calibration of the thermal desorption method ...31

Annex E (informative) Practical example for the calibration of the solvent extraction

method using Florisil® ..........................................................................................................................................................................33

Annex F (informative) Practical example for the gas chromatography with thermal desorption ....35

© ISO 2017 – All rights reserved iii
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ISO 16000-33:2017(E)
Annex G (informative) Practical example for the gas chromatography following

solvent extraction .............................................................................................................................................................................................36

Annex H (informative) Problems related to the blank values .................................................................................................37

Annex I (informative) Example of a sampling protocol ..................................................................................................................38

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

iv © ISO 2017 – All rights reserved
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ISO 16000-33:2017(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: w w w . i s o .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.
© ISO 2017 – All rights reserved v
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ISO 16000-33:2017(E)
Introduction

The different parts of ISO 16000 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 measurement procedures themselves (see Foreword).

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

it-yourself (DIY) rooms, sports rooms and cellars, kitchens and bathrooms], workrooms or workplaces

in buildings which are not subject to health and safety inspections with respect to air pollutants (e.g.

offices, salesrooms), public buildings (e.g. restaurants, theatres, cinemas and other meeting rooms) and

passenger cabins of motor vehicles and public transport are among the most important types of indoor

environment.

Phthalates, the diesters of the ortho-phthalic acid (1,2-benzene dicarbon acid), are emitted into the

indoor air primarily from articles of daily use made of soft polyvinyl chloride (PVC). Typically, phthalates

are used as plasticizers in soft PVC. The five most frequently used phthalates are diisodecylphthalate

(DiDP), diisononylphthalate (DiNP), di(2-ethylhexyl)-phthalate (DEHP), di-n-butyl-phthalate (DBP),

and benzyl-n-butyl-phthalate (BBP). An overview of the most important phthalates, their acronyms and

several relevant substance properties can be found in Table A.1. These phthalates can be determined

in indoor environments by means of the analytical methods incorporating gas chromatography/mass

spectrometry specified in this document.
vi © ISO 2017 – All rights reserved
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INTERNATIONAL STANDARD ISO 16000-33:2017(E)
Indoor air —
Part 33:
Determination of phthalates with gas chromatography/
mass spectrometry (GC/MS)
1 Scope

This document specifies the sampling and analysis of phthalates in indoor air and describes the

sampling and analysis of phthalates in house dust and in solvent wipe samples of surfaces by means of

gas chromatography/mass spectrometry.

Two alternative sampling and processing methods, whose comparability has been proven in a round

[4]

robin test, are specified for indoor air . Sampling can take place using sorbent tubes with subsequent

thermal desorption and GC-MS analysis. Alternatively, sampling can take on other types of sorbent

tubes that are subsequently analysed by solvent extraction with GC-MS.

Depending on the sampling method, the compounds dimethyl phthalate to diisoundecylphthalate

[8]

can be analysed in house dust as described in Annex C . The investigation of house dust samples is

only appropriate as a screening method. This investigation only results in indicative values and is not

acceptable for a final assessment of a potential need for action.

Dimethyl phthalate to diisoundecylphthalate can be analysed in solvent wipe samples as described in

Annex B. Solvent wipe samples are suitable for non-quantitative source identification.

NOTE In principle, the method is also suitable for the analysis of other phthalates, adipates and cyclohexane

dicarboxylic acid esters, but this is confirmed by determination of the performance characteristics in each case.

General information on phthalates are given in Annex A.
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 16000-6:2011, Indoor air — Part 6: Determination of volatile organic compounds in indoor and test

chamber air by active sampling on Tenax TA sorbent, thermal desorption and gas chromatography using

MS or MS-FID
3 Terms and definitions
No terms and definitions are listed in this document.

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

— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org/
© ISO 2017 – All rights reserved 1
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ISO 16000-33:2017(E)
4 Sampling methods and analytical apparatus
4.1 General

Sampling of indoor air takes place either by adsorption on a thermal desorption tube filled with quartz

1) 2) [4][5]

wool and Tenax® TA or on adsorbents such as Florisil® with subsequent solvent extraction . The

quantity of solvent used for solvent extraction procedures should be minimized in order to minimize

blank values. All apparatus and reagents used should be clean, i.e. without detectable quantities of the

compounds of interest.

The experiences from the round robin test have indicated that significant blank value differences can

also be introduced by the solvent. Each new bottle of solvent shall therefore be tested for phthalate

[4]
contamination before use .

NOTE The experiences from the round robin test have indicated that rinsing with clean solvent (no detectable

phthalates) is sufficient to remove contamination from the apparatus and that a sterilization by heating with

subsequent deactivation of the heated glass apparatus is not mandatory.

The ubiquitous distribution of phthalates shall be considered during sampling of indoor air in order

to avoid contamination of the sample. The measures to be considered for blank value minimization,

as well as the advantages and disadvantages of the individual methods, are described in detail in the

respective clauses. Further hints to quality assurance and problems related to blank values that shall

be considered are listed in Clause 10.
4.2 Sampling by adsorption with subsequent thermal desorption

Use the apparatus, reagents and materials described in ISO 16000-6 (including the informative annex

on semi-volatile compounds) with the following additional specific requirements:
4.2.1 Apparatus, operating materials and chemicals

4.2.1.1 Thermal desorption tube, stainless steel, inert-coated steel or glass tube filled with a 1 cm

loosely packed plug of non-friable quartz wool backed up by at least 200 mg of adsorbent, e.g. Tenax®

TA 20/35 (see ISO 16000-6:2011, Annex D).
4.2.1.2 Sampling system, according to Figure 1.

4.2.1.3 Pump, suitable for a volume flow in the range 50 ml/min to 200 ml/min under the sampling

conditions; recommended sampling volume of approximately 20 l to approximately 70 l.

4.2.1.4 Gas volume meter, the maximal measurement inaccuracy shall not exceed 5 %.

4.2.1.5 Laboratory sampling facilities, hygrometer, thermometer, barometer.

4.2.1.6 Internal standards, required as quality control measure of the whole analytical process

including sampling; suitable examples include: the ring-deuterated compounds D4-DMP, D4-DEP, D4-

DBP, D4-BBP, D4-DEHP, D4-DOP as well as the non-deuterated diallyl phthalate (DAlP), see Clause 5 and

Table 3. Standards shall be prepared in phthalate-free methanol, as described in ISO 16000-6, at a level

such that a maximum 1 µl injection introduces approximately the same mass of analyte onto the sampling

end of the tubes as is expected to be collected during sampling.

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

of the 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) Florisil® is the trade name of product supplied by U.S. Silica. This information is given for the convenience of the

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 © ISO 2017 – All rights reserved
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ISO 16000-33:2017(E)

4.2.1.7 Thermal desorption unit, coupled to GC-MS for the two-stage thermal desorption of the

sorbent tubes and transfer of desorbed vapours via an inert gas flow into a gas chromatographic (GC)

system, fitted with a mass spectrometric (MS) detector.

NOTE Deactivated (silanised) glass wool or quartz wool can also be used as adsorbent after an appropriate

method validation.
4.2.2 Preparation of the thermal desorption tube

The use of a tube packed with quartz wool and Tenax® TA presupposes knowledge of ISO 16000-6.

Prepacked and preconditioned sorbent tubes are available commercially or can be prepared in the

laboratory as follows:

A plug of non-friable quartz wool, usually supported by a stainless steel mesh, is inserted at the

sampling end of the tube. The required mass of sorbent is poured into the tube behind the quartz wool

plug. The far end of the sorbent bed is typically supported by a second plug of quartz wool or a stainless

steel mesh.

A minimum of 200 mg sorbent shall be used per tube in order to guarantee the sorption capacity.

NOTE Determination of the breakthrough volume is described in ISO 16017-1:2000, Annex B. The

breakthrough volumes are proportional to the dimensions and masses of the sorbents. The rule of the thumb is

that the guaranteed sample volume doubles itself when the sorbent bed length is doubled (while retaining the

tube diameter).

After filling of the thermal desorption tubes (e.g. with Tenax® TA ), the tubes are conditioned

for approximately 8 h at 280 °C followed by approximately 30 min at 300 °C in an inert gas flow

(100 ml/min). The purified sorption tubes are closed and stored at room temperature and in the dark in

a container that prevents sample contamination.

Analyse a representative number of conditioned tubes for blank value, using routine analytical

parameters, to ensure that thermal desorption blank is sufficiently small (see ISO 16000-6:2011, 7.1).

Sampling should take place as soon as possible after conditioning. If sampling is not possible

within approximately 14 days after conditioning, then the tube shall be reconditioned for 15 min at

approximately 300 °C before sampling. In order to avoid contamination, the thermal desorption tubes

should be touched only with cotton gloves. In addition, labelling shall be omitted.

The thermal desorption device should ensure that any contamination from external tube surfaces is

excluded from the analytical sample flow path. If the selected analytical system does not do this, tubes

shall only be handled using clean cotton gloves, in the field and laboratory, to minimize contamination.

Tubes should be indelibly and individually labelled but without attaching adhesive labels which might

jam or discolour during thermal desorption.
4.2.3 Sampling

Prior to sampling, the conditioned tubes are spiked with a maximum of 1 µl internal standard solution

in methanol (e.g. 20 ng/µl for a sampling volume of 50 l; the absolute mass of the additionally spiked

standard depends on the sampling volume and the operating range of the method). The standard

solution is usually applied on the sampling end of the sorbent tube.

The sampling equipment is assembled according to Figure 1 and shall be free of leaks. The

pump is connected to the non-sampling end of the sorbent tube by means of polyethylene or

polytetrafluoroethylene (PTFE) connectors and is switched on. If the breakthrough volume of the

analysed phthalates is unknown, then two sorption tubes shall be connected in series. The tubes shall

be connected with a phthalate-free coupling.

The volume flow, as well as the temperature, the absolute air pressure and the relative air humidity,

shall be recorded. The suitable sampling volume flows are within the range of 50 ml/min to 200 ml/min.

This corresponds to a recommended sampling volume of approximately 20 l to 70 l for a sampling

© ISO 2017 – All rights reserved 3
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ISO 16000-33:2017(E)

duration of approximately 2 h to 24 h. After sampling, the sorption tube is removed from the sampling

equipment; both ends of the sorption tube shall be closed.
A duplicate sampling of the indoor air is recommended.

Sampled tubes shall be transported to the laboratory and analysed as soon as possible.

4.3 Sampling by adsorption and subsequent solvent extraction
4.3.1 Apparatus, operating materials and chemicals
4.3.1.1 Sampling system, according to Figure 1.

4.3.1.2 Pump, suitable for a volume flow of approximately 2 l/min under the conditions of the

3 3

sampling, recommended sampling volume of approximately 1 m to 3 m in 8 h to 24 h.

4.3.1.3 Gas volume meter, the maximal measurement inaccuracy shall not exceed 5 %.

4.3.1.4 Muffle furnace.
4.3.1.5 Flat, heat resistant evaporating dish, for heating Florisil® .
4.3.1.6 Florisil® , 60 to 100 mesh.
4.3.1.7 Glass wool, silanized.

4.3.1.8 Glass flask, with screw-cap and polytetrafluoroethylene (PTFE) sealing, 50 ml.

4.3.1.9 Adsorption tubes, glass tube, approximately 200 mm long, internal diameter approximately

10 mm to 12 mm.
4.3.1.10 Laboratory sampling facilities, hygrometer, thermometer, barometer.

4.3.1.11 Solvent, e.g. tertiary butyl methyl ether (TBME) or toluene, free of blank values (solvent shall

be tested for the absence of phthalate blank values).

4.3.1.12 Internal standards, suitable are, e.g. the ring-deuterated compounds D4-DMP, D4-DEP, D4-

DBP, D4-BBP, D4-DEHP, D4-DOP as well as the non-deuterated diallyl phthalate (DAlP); see Clause 5 and

Table 3.
4 © ISO 2017 – All rights reserved
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ISO 16000-33:2017(E)

4.3.1.13 GC-MS, gas chromatographic (GC) system, fitted with a mass spectrometric (MS) detector.

Key
1 sampling tube
2 membrane vacuum pump
3 timer switch (optional)
4 anti-abrasion filter
5 volume measuring device or mass flow controller
6 protective housing
Figure 1 — Schematic diagram of the sampling equipment
Figure 2 — Filling of the glass tube
Key
1 Florisil®
2 glass wool
4.3.2 Preparation of Florisil® and the adsorption tubes

Florisil® is spread out in a thin layer (approximately 3 cm to 4 cm) on an evaporation dish and

heated at 800 °C for 6 h. After cooling down in the desiccator it is deactivated with bi-distilled water

(3 % proportion by mass). To this end, 5 g Florisil® and 150 µl water are given to a 50 ml glass flask

with a screw-cap and polytetrafluoroethylene (PTFE) sealing. After closing the flask, Florisil®

shall be mixed for approximately 45 min until a uniformly flowing powder has formed again. The

deactivated Florisil® is then filled into an adsorption tube (see Figure 2). The filling height should be

© ISO 2017 – All rights reserved 5
---------------------- Page: 11 ----------------------
ISO 16000-33:2017(E)

approximately 10 cm to 13 cm. The ends of the Florisil® filling are closed with silanised glass wool.

The filled tubes are stored in the desiccator over silica gel until air sampling.

[15]
NOTE The geometry of the tube is based on the DFG method .
4.3.3 Hints to the application of Florisil®

Each charge of Florisil® newly heated and deactivated according to 4.3.2 shall be examined for blank

values. Charges where high phthalate blank values are still measured after such treatment shall be

heated and deactivated anew.

As long as the prepared tubes are stored in the desiccator, they are suitable for storage and use within

up to six months. After expiration of this period, unused tubes shall be emptied and the Florisil® shall

be treated again according to 4.3.2.

Other adsorbents such as Chromosorb 106 or comparable carrier materials can be utilized as adsorption

agents. Adsorbent preparation and sampling shall then be modified accordingly, and the suitability

shall be proven by a determination of the performance characteristics.
4.3.4 Sampling

A defined volume (e.g. 10 µl) of the internal standard solution (e.g. 100 mg/l, this corresponds to an

absolute mass of the internal standard of 1 µg) shall be added prior to sampling. The preparation of

the solutions of the internal standards is described in Annex D (for thermal desorption method) and in

Annex E (for solvent extraction method using Florisil® ).

The internal standard is added (typically) by means of a microlitre syringe. The standard solution is

usually placed on the adsorbent on the side oriented towards the flow. The amount to be added for the

3 3

anticipated operating ranges from 0,05 µg/m to 10 µg/m is listed in Table 1. The compounds listed in

Clause 5 are suitable as internal standards.

Table 1 — Operating range for determination of phthalates with contents from 0,05 µg/m to

10 µg/m in an air sample
Concentration of the Corresponds to a
reduced sampling concentration in the air
solution
mg/l µg/m
0,05 0,05
0,1 0,1
0,5 0,5
1,0 1,0
2,5 2,5
5,0 5,0
10,0 10,0
The data concerning the calculated concentrations in the air
are tentative. The actual detection and quantification limits of
the method shall be determined by the test laboratory based
on the calibration under consideration of the blank value.
NOTE The data given in Table 1 are valid for an air volume
of 1 m and a sample processing as described in 4.3.5.

The sampling equipment is assembled according to Figure 1 and a leak test is performed. The volume

flow, as well as the temperature, the absolute air pressure and the relative air humidity, shall be

recorded. Sampling takes place by means of a pump, and the sampling volume amounts to 1 m to

3) DFG stands for Deutsche Forschungsgemeinschaft, i.e. the German Research Foundation.

6 © ISO 2017 – All rights reserved
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ISO 1
...

SLOVENSKI STANDARD
SIST ISO 16000-33:2019
01-september-2019
Notranji zrak - 33. del: Določevanje ftalatov s plinsko kromatografijo/masno
spektrometrijo (GC/MS)
Indoor air - Part 33: Determination of phthalates with gas chromatography/mass
spectrometry (GC/MS)

Air intérieur - Partie 33: Détermination des phthalates par chromatographie en phase

gazeuse/spectrométrie de masse (CPG/SM)
Ta slovenski standard je istoveten z: ISO 16000-33:2017
ICS:
13.040.20 Kakovost okoljskega zraka Ambient atmospheres
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
SIST ISO 16000-33:2019 en

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

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SIST ISO 16000-33:2019
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SIST ISO 16000-33:2019
INTERNATIONAL ISO
STANDARD 16000-33
First edition
2017-08
Indoor air —
Part 33:
Determination of phthalates with gas
chromatography/mass spectrometry
(GC/MS)
Air intérieur —
Partie 33: Détermination des phthalates par chromatographie en
phase gazeuse/spectrométrie de masse (CPG/SM)
Reference number
ISO 16000-33:2017(E)
ISO 2017
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SIST ISO 16000-33:2019
ISO 16000-33:2017(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2017, Published in Switzerland

All rights reserved. Unless otherwise specified, 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
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. +41 22 749 01 11
Fax +41 22 749 09 47
copyright@iso.org
www.iso.org
ii © ISO 2017 – All rights reserved
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SIST ISO 16000-33:2019
ISO 16000-33:2017(E)
Contents Page

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

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

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

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

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

4 Sampling methods and analytical apparatus .......................................................................................................................... 2

4.1 General ........................................................................................................................................................................................................... 2

4.2 Sampling by adsorption with subsequent thermal desorption .................................................................... 2

4.2.1 Apparatus, operating materials and chemicals ..................................................................................... 2

4.2.2 Preparation of the thermal desorption tube ............................................................................................ 3

4.2.3 Sampling.................................................................................................................................................................................. 3

4.3 Sampling by adsorption and subsequent solvent extraction .......................................................................... 4

4.3.1 Apparatus, operating materials and chemicals ..................................................................................... 4

4.3.2 Preparation of Florisil® and the adsorption tubes ....................................................................... 5

2) 6

4.3.3 Hints to the application of Florisil® ............................................................................................................

4.3.4 Sampling.................................................................................................................................................................................. 6

4.3.5 Sample conditioning ..................................................................................................................................................... 7

5 Calibration .................................................................................................................................................................................................................. 7

5.1 General ........................................................................................................................................................................................................... 7

5.2 Calibration of the thermal desorption method ........................................................................................................... 8

5.3 Calibration of the solvent extraction method ............................................................................................................... 8

6 Identification and quantification ........................................................................................................................................................ 8

6.1 Mass spectrometric analysis ....................................................................................................................................................... 8

7 Establishment of calibration curves and calculation of the analyte mass .............................................14

7.1 Establishment of calibration curves ..................................................................................................................................14

7.2 Calculation of the analyte mass .............................................................................................................................................14

8 Calculation of indoor air concentrations .................................................................................................................................15

9 Performance characteristics .................................................................................................................................................................16

9.1 Detection limit ......................................................................................................................................................................................16

9.2 Quantification limit and problems related to the blank values ..................................................................16

9.3 Reproducibility standard deviation and repeatability standard deviation .....................................17

10 Quality assurance .............................................................................................................................................................................................19

10.1 Method verification and determination of blanks .................................................................................................19

10.1.1 Field blank value of the indoor air.................................................................................................................19

10.1.2 Analytical laboratory blank value ..................................................................................................................19

10.2 Measures for blank value minimization .........................................................................................................................19

10.3 Documents ...............................................................................................................................................................................................20

11 Interferences .........................................................................................................................................................................................................20

Annex A (informative) General information on phthalates .......................................................................................................21

Annex B (informative) Screening phthalates in solvent wipe tests ...................................................................................24

Annex C (informative) Screening phthalates in house dust .......................................................................................................27

Annex D (informative) Practical example for the calibration of the thermal desorption method ...31

Annex E (informative) Practical example for the calibration of the solvent extraction

method using Florisil® ..........................................................................................................................................................................33

Annex F (informative) Practical example for the gas chromatography with thermal desorption ....35

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Annex G (informative) Practical example for the gas chromatography following

solvent extraction .............................................................................................................................................................................................36

Annex H (informative) Problems related to the blank values .................................................................................................37

Annex I (informative) Example of a sampling protocol ..................................................................................................................38

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

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SIST ISO 16000-33:2019
ISO 16000-33:2017(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: w w w . i s o .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.
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Introduction

The different parts of ISO 16000 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 measurement procedures themselves (see Foreword).

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

it-yourself (DIY) rooms, sports rooms and cellars, kitchens and bathrooms], workrooms or workplaces

in buildings which are not subject to health and safety inspections with respect to air pollutants (e.g.

offices, salesrooms), public buildings (e.g. restaurants, theatres, cinemas and other meeting rooms) and

passenger cabins of motor vehicles and public transport are among the most important types of indoor

environment.

Phthalates, the diesters of the ortho-phthalic acid (1,2-benzene dicarbon acid), are emitted into the

indoor air primarily from articles of daily use made of soft polyvinyl chloride (PVC). Typically, phthalates

are used as plasticizers in soft PVC. The five most frequently used phthalates are diisodecylphthalate

(DiDP), diisononylphthalate (DiNP), di(2-ethylhexyl)-phthalate (DEHP), di-n-butyl-phthalate (DBP),

and benzyl-n-butyl-phthalate (BBP). An overview of the most important phthalates, their acronyms and

several relevant substance properties can be found in Table A.1. These phthalates can be determined

in indoor environments by means of the analytical methods incorporating gas chromatography/mass

spectrometry specified in this document.
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SIST ISO 16000-33:2019
INTERNATIONAL STANDARD ISO 16000-33:2017(E)
Indoor air —
Part 33:
Determination of phthalates with gas chromatography/
mass spectrometry (GC/MS)
1 Scope

This document specifies the sampling and analysis of phthalates in indoor air and describes the

sampling and analysis of phthalates in house dust and in solvent wipe samples of surfaces by means of

gas chromatography/mass spectrometry.

Two alternative sampling and processing methods, whose comparability has been proven in a round

[4]

robin test, are specified for indoor air . Sampling can take place using sorbent tubes with subsequent

thermal desorption and GC-MS analysis. Alternatively, sampling can take on other types of sorbent

tubes that are subsequently analysed by solvent extraction with GC-MS.

Depending on the sampling method, the compounds dimethyl phthalate to diisoundecylphthalate

[8]

can be analysed in house dust as described in Annex C . The investigation of house dust samples is

only appropriate as a screening method. This investigation only results in indicative values and is not

acceptable for a final assessment of a potential need for action.

Dimethyl phthalate to diisoundecylphthalate can be analysed in solvent wipe samples as described in

Annex B. Solvent wipe samples are suitable for non-quantitative source identification.

NOTE In principle, the method is also suitable for the analysis of other phthalates, adipates and cyclohexane

dicarboxylic acid esters, but this is confirmed by determination of the performance characteristics in each case.

General information on phthalates are given in Annex A.
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 16000-6:2011, Indoor air — Part 6: Determination of volatile organic compounds in indoor and test

chamber air by active sampling on Tenax TA sorbent, thermal desorption and gas chromatography using

MS or MS-FID
3 Terms and definitions
No terms and definitions are listed in this document.

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

— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org/
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4 Sampling methods and analytical apparatus
4.1 General

Sampling of indoor air takes place either by adsorption on a thermal desorption tube filled with quartz

1) 2) [4][5]

wool and Tenax® TA or on adsorbents such as Florisil® with subsequent solvent extraction . The

quantity of solvent used for solvent extraction procedures should be minimized in order to minimize

blank values. All apparatus and reagents used should be clean, i.e. without detectable quantities of the

compounds of interest.

The experiences from the round robin test have indicated that significant blank value differences can

also be introduced by the solvent. Each new bottle of solvent shall therefore be tested for phthalate

[4]
contamination before use .

NOTE The experiences from the round robin test have indicated that rinsing with clean solvent (no detectable

phthalates) is sufficient to remove contamination from the apparatus and that a sterilization by heating with

subsequent deactivation of the heated glass apparatus is not mandatory.

The ubiquitous distribution of phthalates shall be considered during sampling of indoor air in order

to avoid contamination of the sample. The measures to be considered for blank value minimization,

as well as the advantages and disadvantages of the individual methods, are described in detail in the

respective clauses. Further hints to quality assurance and problems related to blank values that shall

be considered are listed in Clause 10.
4.2 Sampling by adsorption with subsequent thermal desorption

Use the apparatus, reagents and materials described in ISO 16000-6 (including the informative annex

on semi-volatile compounds) with the following additional specific requirements:
4.2.1 Apparatus, operating materials and chemicals

4.2.1.1 Thermal desorption tube, stainless steel, inert-coated steel or glass tube filled with a 1 cm

loosely packed plug of non-friable quartz wool backed up by at least 200 mg of adsorbent, e.g. Tenax®

TA 20/35 (see ISO 16000-6:2011, Annex D).
4.2.1.2 Sampling system, according to Figure 1.

4.2.1.3 Pump, suitable for a volume flow in the range 50 ml/min to 200 ml/min under the sampling

conditions; recommended sampling volume of approximately 20 l to approximately 70 l.

4.2.1.4 Gas volume meter, the maximal measurement inaccuracy shall not exceed 5 %.

4.2.1.5 Laboratory sampling facilities, hygrometer, thermometer, barometer.

4.2.1.6 Internal standards, required as quality control measure of the whole analytical process

including sampling; suitable examples include: the ring-deuterated compounds D4-DMP, D4-DEP, D4-

DBP, D4-BBP, D4-DEHP, D4-DOP as well as the non-deuterated diallyl phthalate (DAlP), see Clause 5 and

Table 3. Standards shall be prepared in phthalate-free methanol, as described in ISO 16000-6, at a level

such that a maximum 1 µl injection introduces approximately the same mass of analyte onto the sampling

end of the tubes as is expected to be collected during sampling.

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

of the 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) Florisil® is the trade name of product supplied by U.S. Silica. This information is given for the convenience of the

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.
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4.2.1.7 Thermal desorption unit, coupled to GC-MS for the two-stage thermal desorption of the

sorbent tubes and transfer of desorbed vapours via an inert gas flow into a gas chromatographic (GC)

system, fitted with a mass spectrometric (MS) detector.

NOTE Deactivated (silanised) glass wool or quartz wool can also be used as adsorbent after an appropriate

method validation.
4.2.2 Preparation of the thermal desorption tube

The use of a tube packed with quartz wool and Tenax® TA presupposes knowledge of ISO 16000-6.

Prepacked and preconditioned sorbent tubes are available commercially or can be prepared in the

laboratory as follows:

A plug of non-friable quartz wool, usually supported by a stainless steel mesh, is inserted at the

sampling end of the tube. The required mass of sorbent is poured into the tube behind the quartz wool

plug. The far end of the sorbent bed is typically supported by a second plug of quartz wool or a stainless

steel mesh.

A minimum of 200 mg sorbent shall be used per tube in order to guarantee the sorption capacity.

NOTE Determination of the breakthrough volume is described in ISO 16017-1:2000, Annex B. The

breakthrough volumes are proportional to the dimensions and masses of the sorbents. The rule of the thumb is

that the guaranteed sample volume doubles itself when the sorbent bed length is doubled (while retaining the

tube diameter).

After filling of the thermal desorption tubes (e.g. with Tenax® TA ), the tubes are conditioned

for approximately 8 h at 280 °C followed by approximately 30 min at 300 °C in an inert gas flow

(100 ml/min). The purified sorption tubes are closed and stored at room temperature and in the dark in

a container that prevents sample contamination.

Analyse a representative number of conditioned tubes for blank value, using routine analytical

parameters, to ensure that thermal desorption blank is sufficiently small (see ISO 16000-6:2011, 7.1).

Sampling should take place as soon as possible after conditioning. If sampling is not possible

within approximately 14 days after conditioning, then the tube shall be reconditioned for 15 min at

approximately 300 °C before sampling. In order to avoid contamination, the thermal desorption tubes

should be touched only with cotton gloves. In addition, labelling shall be omitted.

The thermal desorption device should ensure that any contamination from external tube surfaces is

excluded from the analytical sample flow path. If the selected analytical system does not do this, tubes

shall only be handled using clean cotton gloves, in the field and laboratory, to minimize contamination.

Tubes should be indelibly and individually labelled but without attaching adhesive labels which might

jam or discolour during thermal desorption.
4.2.3 Sampling

Prior to sampling, the conditioned tubes are spiked with a maximum of 1 µl internal standard solution

in methanol (e.g. 20 ng/µl for a sampling volume of 50 l; the absolute mass of the additionally spiked

standard depends on the sampling volume and the operating range of the method). The standard

solution is usually applied on the sampling end of the sorbent tube.

The sampling equipment is assembled according to Figure 1 and shall be free of leaks. The

pump is connected to the non-sampling end of the sorbent tube by means of polyethylene or

polytetrafluoroethylene (PTFE) connectors and is switched on. If the breakthrough volume of the

analysed phthalates is unknown, then two sorption tubes shall be connected in series. The tubes shall

be connected with a phthalate-free coupling.

The volume flow, as well as the temperature, the absolute air pressure and the relative air humidity,

shall be recorded. The suitable sampling volume flows are within the range of 50 ml/min to 200 ml/min.

This corresponds to a recommended sampling volume of approximately 20 l to 70 l for a sampling

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duration of approximately 2 h to 24 h. After sampling, the sorption tube is removed from the sampling

equipment; both ends of the sorption tube shall be closed.
A duplicate sampling of the indoor air is recommended.

Sampled tubes shall be transported to the laboratory and analysed as soon as possible.

4.3 Sampling by adsorption and subsequent solvent extraction
4.3.1 Apparatus, operating materials and chemicals
4.3.1.1 Sampling system, according to Figure 1.

4.3.1.2 Pump, suitable for a volume flow of approximately 2 l/min under the conditions of the

3 3

sampling, recommended sampling volume of approximately 1 m to 3 m in 8 h to 24 h.

4.3.1.3 Gas volume meter, the maximal measurement inaccuracy shall not exceed 5 %.

4.3.1.4 Muffle furnace.
4.3.1.5 Flat, heat resistant evaporating dish, for heating Florisil® .
4.3.1.6 Florisil® , 60 to 100 mesh.
4.3.1.7 Glass wool, silanized.

4.3.1.8 Glass flask, with screw-cap and polytetrafluoroethylene (PTFE) sealing, 50 ml.

4.3.1.9 Adsorption tubes, glass tube, approximately 200 mm long, internal diameter approximately

10 mm to 12 mm.
4.3.1.10 Laboratory sampling facilities, hygrometer, thermometer, barometer.

4.3.1.11 Solvent, e.g. tertiary butyl methyl ether (TBME) or toluene, free of blank values (solvent shall

be tested for the absence of phthalate blank values).

4.3.1.12 Internal standards, suitable are, e.g. the ring-deuterated compounds D4-DMP, D4-DEP, D4-

DBP, D4-BBP, D4-DEHP, D4-DOP as well as the non-deuterated diallyl phthalate (DAlP); see Clause 5 and

Table 3.
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4.3.1.13 GC-MS, gas chromatographic (GC) system, fitted with a mass spectrometric (MS) detector.

Key
1 sampling tube
2 membrane vacuum pump
3 timer switch (optional)
4 anti-abrasion filter
5 volume measuring device or mass flow controller
6 protective housing
Figure 1 — Schematic diagram of the sampling equipment
Figure 2 — Filling of the glass tube
Key
1 Florisil®
2 glass wool
4.3.2 Preparation of Florisil® and the adsorption tubes

Florisil® is spread out in a thin layer (approximately 3 cm to 4 cm) on an evaporation dish and

heated at 800 °C for 6 h. After cooling down in the desiccator it is deactivated with bi-distilled water

(3 % proportion by mass). To this end, 5 g Florisil® and 150 µl water are given to a 50 ml glass flask

with a screw-cap and polytetrafluoroethylene (PTFE) sealing. After closing the flask, Florisil®

shall be mixed for approximately 45 min until a uniformly flowing powder has formed again. The

deactivated Florisil® is then filled into an adsorption tube (see Figure 2). The filling height should be

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approximately 10 cm to 13 cm. The ends of the Florisil® filling are closed with silanised glass wool.

The filled tubes are stored in the desiccator over silica gel until air sampling.

[15]
NOTE The geometry of the tube is based on the DFG method .
4.3.3 Hints to the application of Florisil®

Each charge of Florisil® newly heated and deactivated according to 4.3.2 shall be examined for blank

values. Charges where high phthalate blank values are still measured after such treatment shall be

heated and deactivated anew.

As long as the prepared tubes are stored in the desiccator, they are suitable for storage and use within

up to six months. After expiration of this period, unused tubes shall be emptied and the Florisil® shall

be treated again according to 4.3.2.

Other adsorbents such as Chromosorb 106 or comparable carrier materials can be utilized as adsorption

agents. Adsorbent preparation and sampling shall then be modified accordingly, and the suitability

shall be proven by a determination of the performance characteristics.
4.3.4 Sampling

A defined volume (e.g. 10 µl) of the internal standard solution (e.g. 100 mg/l, this corresponds to an

absolute mass of the internal standard of 1 µg) shall be added prior to sampling. The preparation of

the solutions of the internal standards is described in Annex D (for thermal desorption method) and in

Annex E (for solvent extraction method using Florisil® ).

The internal standard is added (typically) by means of a microlitre syringe. The standard solution is

usually placed on the adsorbent on the side oriented towards the flow. The amount to be added for the

3 3

anticipated operating ranges from 0,05 µg/m to 10 µg/m is listed in Table 1. The compounds listed in

Clause 5 are s
...

NORME ISO
INTERNATIONALE 16000-33
Première édition
2017-08
Air intérieur —
Partie 33:
Détermination des phthalates par
chromatographie en phase gazeuse/
spectrométrie de masse (CPG/SM)
Indoor air —
Part 33: Determination of phthalates with gas chromatography/mass
spectrometry (GC/MS)
Numéro de référence
ISO 16000-33:2017(F)
ISO 2017
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ISO 16000-33:2017(F)
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Tel. +41 22 749 01 11
Fax +41 22 749 09 47
copyright@iso.org
www.iso.org
ii © ISO 2017 – Tous droits réservés
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ISO 16000-33:2017(F)
Sommaire Page

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

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

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

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

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

4 Méthodes de prélèvement et appareillage d’analyse ..................................................................................................... 2

4.1 Généralités .................................................................................................................................................................................................. 2

4.2 Prélèvement par adsorption suivie d’une désorption thermique .............................................................. 2

4.2.1 Appareillage, matériaux et produits chimiques .................................................................................... 2

4.2.2 Préparation du tube de désorption thermique ..................................................................................... 3

4.2.3 Prélèvement ......................................................................................................................................................................... 3

4.3 Prélèvement par adsorption suivie d’une extraction au solvant ................................................................. 4

4.3.1 Appareillage, matériels et produits chimiques ...................................................................................... 4

4.3.2 Préparation du Florisil® et des tubes d’adsorption ..................................................................... 5

2) 6

4.3.3 Recommandations concernant l’utilisation de Florisil® ..........................................................

4.3.4 Prélèvement ......................................................................................................................................................................... 6

4.3.5 Conditionnement des échantillons .................................................................................................................. 7

5 Étalonnage .................................................................................................................................................................................................................. 7

5.1 Généralités .................................................................................................................................................................................................. 7

5.2 Étalonnage de la méthode de désorption thermique ............................................................................................ 8

5.3 Étalonnage de la méthode d’extraction au solvant .................................................................................................. 8

6 Identification et quantification ............................................................................................................................................................. 8

6.1 Analyse par spectrométrie de masse ................................................................................................................................... 8

7 Établissement des courbes d’étalonnage et calcul de la masse d’analyte .............................................14

7.1 Établissement des courbes d’étalonnage ......................................................................................................................14

7.2 Calcul de la masse d’analyte .....................................................................................................................................................14

8 Calcul des concentrations dans l’air intérieur ...................................................................................................................16

9 Performance de la méthode ...................................................................................................................................................................16

9.1 Limite de détection ...........................................................................................................................................................................16

9.2 Limite de quantification et problèmes liés aux valeurs de blanc .............................................................16

9.3 Écart-type de reproductibilité et écart-type de répétabilité ........................................................................17

10 Assurance de la qualité ...............................................................................................................................................................................19

10.1 Vérification de la méthode et détermination des blancs .................................................................................19

10.1.1 Valeur de blanc de terrain de l’air intérieur ..........................................................................................19

10.1.2 Valeur de blanc de laboratoire d’analyse .................................................................................................19

10.2 Mesures permettant de réduire les valeurs de blanc .........................................................................................19

10.3 Documents ...............................................................................................................................................................................................20

11 Interférences .........................................................................................................................................................................................................20

Annexe A (informative) Informations générales sur les phtalates ....................................................................................21

Annexe B (informative) Recherche des phtalates lors de prélèvements de surface ........................................25

Annexe C (informative) Recherche des phtalates dans les poussières domestiques ......................................28

Annexe D (informative) Exemple pratique pour l’étalonnage de la méthode

de désorption thermique..........................................................................................................................................................................32

Annexe E (informative) Exemple pratique pour l’étalonnage de la méthode d’extraction

au solvant en utilisant du Florisil® .........................................................................................................................................34

Annexe F (informative) Exemple pratique pour la chromatographie en phase gazeuse avec

désorption thermique..................................................................................................................................................................................36

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ISO 16000-33:2017(F)
Annexe G (informative) Exemple pratique pour la chromatographie en phase gazeuse

couplée à une extraction au solvant ..............................................................................................................................................37

Annexe H (informative) Problèmes liés aux valeurs de blanc.................................................................................................38

Annexe I (informative) Exemple de protocole d’échantillonnage .......................................................................................39

Bibliographie ...........................................................................................................................................................................................................................40

iv © ISO 2017 – Tous droits réservés
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ISO 16000-33:2017(F)
Avant-propos

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

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

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

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

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

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

concerne la normalisation électrotechnique.

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

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

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

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

.iso .org/ directives).

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

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

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

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

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

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

Les appellations commerciales éventuellement mentionnées dans le présent document sont données

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

engagement.

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

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

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

techniques au commerce (OTC), voir le lien suivant: w w w . i s o .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.

Une liste de toutes les parties de la série de normes ISO 16000 peut être consultée sur le site de l’ISO.

© ISO 2017 – Tous droits réservés v
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ISO 16000-33:2017(F)
Introduction

Les différentes parties de l’ISO 16000 décrivent les exigences générales s’appliquant au mesurage des

polluants de l’air intérieur et les conditions importantes à observer avant et pendant le prélèvement

de polluants individuels ou de groupes de polluants, ainsi que les modes opératoires de mesurage

proprement dits (voir l’Avant-propos).

La définition de l’environnement intérieur est donnée par l’ISO 16000-1. Les logements [salles de séjour,

chambres à coucher, ateliers de bricolage, salles de sport, caves, cuisines et salles de bain], les salles ou

lieux de travail dans les bâtiments qui ne sont pas soumis à des inspections d’hygiène et de sécurité

concernant les polluants de l’air intérieur (par exemple bureaux, locaux de vente), les bâtiments publics

(par exemple restaurants, théâtres, cinémas et autres salles de réunion) et les habitacles des véhicules

à moteur et des transports en commun comptent parmi les types d’ambiance intérieure les plus

importants.

Les phtalates, les diesters de l’acide ortho-phtalique (acide 1,2-benzène dicarbonique), sont émis dans

l’air intérieur principalement par des articles d’usage quotidien constitués de chlorure de polyvinyle

(PVC) souple. Les phtalates sont habituellement utilisés comme plastifiants dans le PVC souple. Les cinq

phtalates les plus fréquemment utilisés sont le phtalate de diisodécyle (DiDP), le phtalate de diisononyle

(DiNP), le phtalate de di(2-éthylhexyle) (DEHP), le phtalate de di-n-butyle (DBP) et le phtalate de

benzyl-n-butyle (BBP). Un aperçu des phtalates les plus importants, de leurs acronymes et de plusieurs

propriétés pertinentes de ces substances est donné dans le Tableau A.1. Ces phtalates peuvent être

déterminés dans les ambiances intérieures par des méthodes d’analyse intégrant la chromatographie

en phase gazeuse/spectrométrie de masse spécifiée dans le présent document.
vi © ISO 2017 – Tous droits réservés
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NORME INTERNATIONALE ISO 16000-33:2017(F)
Air intérieur —
Partie 33:
Détermination des phthalates par chromatographie en
phase gazeuse/spectrométrie de masse (CPG/SM)
1 Domaine d’application

Le présent document spécifie le prélèvement et l’analyse des phtalates dans l’air intérieur et décrit

le prélèvement et l’analyse des phtalates dans des échantillons de poussières domestiques et des

prélèvements de surface (frottis) par chromatographie en phase gazeuse/spectrométrie de masse.

Deux méthodes possibles de prélèvement et de traitement, dont la comparabilité a été démontrée au

[4]

cours d’un essai interlaboratoires, sont spécifiées pour l’air intérieur . Le prélèvement peut être réalisé

à l’aide de tubes à sorbant suivi d’une désorption thermique et d’une analyse par CPG/SM. En variante,

le prélèvement peut être réalisé sur d’autres types de tubes à sorbant qui sont ensuite analysés par

extraction au solvant avec analyse par CPG/SM.

Selon la méthode de prélèvement, les composés phtalate de diméthyle à phtalate de diisoundécyle

[8]

peuvent être analysés dans les poussières domestiques, comme décrit dans l’Annexe C . L’étude

d’échantillons de poussières domestiques est appropriée uniquement comme méthode de diagnostic

rapide. Cette étude donne seulement des valeurs indicatives et n’est pas acceptable pour une évaluation

finale de la nécessité éventuelle d’une action.

Les composés phtalate de diméthyle à phtalate de diisoundécyle peuvent être analysés dans des

frottis comme décrit dans l’Annexe B. Les frottis conviennent pour l’identification non quantitative des

sources.

NOTE En principe, la méthode convient également pour l’analyse d’autres phtalates, adipates et esters d’acide

cyclohexane dicarboxylique, mais cela est confirmé dans chaque cas par la détermination des performances

analytiques.
Des informations générales sur les phtalates sont données dans l’Annexe A.
2 Références normatives

Les documents suivants cités dans le texte 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 16000-6:2011, Air intérieur — Partie 6: Dosage des composés organiques volatils dans l’air intérieur

des locaux et chambres d’essai par échantillonnage actif sur le sorbant Tenax TA, désorption thermique et

chromatographie en phase gazeuse utilisant MS ou MS-FID
3 Termes et définitions
Aucun terme n’est défini dans le présent document.

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

© ISO 2017 – Tous droits réservés 1
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ISO 16000-33:2017(F)
— IEC Electropedia: disponible à l’adresse http:// www .electropedia .org/
4 Méthodes de prélèvement et appareillage d’analyse
4.1 Généralités

Le prélèvement de l’air intérieur est réalisé par adsorption dans un tube de désorption thermique

1) 2)

rempli de laine de quartz ou de Tenax® TA sur des adsorbants tels que le Florisil® suivie d’une

[4][5]

extraction au solvant . Il convient de limiter la quantité de solvant utilisée pour les modes

opératoires d’extraction afin de réduire au minimum les valeurs de blanc. Il convient que l’ensemble de

l’appareillage et des réactifs utilisés soit propre, c’est-à-dire sans quantités détectables des composés

étudiés.

Les expériences réalisées lors de l’essai interlaboratoires ont montré que des écarts significatifs des

valeurs de blanc peuvent également être introduits par le solvant. Chaque nouveau flacon de solvant

[4]

doit donc être soumis à essai avant utilisation afin de déceler toute contamination par les phtalates .

NOTE Les expériences réalisées lors de l’essai interlaboratoires ont montré qu’un rinçage avec un solvant

propre (aucun phtalate détectable) suffit pour éliminer la contamination de l’appareillage et qu’une stérilisation

par la chaleur suivie d’une désactivation de la verrerie chauffée n’est pas obligatoire.

La distribution ubiquiste des phtalates doit être prise en compte pendant le prélèvement de l’air intérieur

pour éviter la contamination de l’échantillon. Les mesures à envisager pour réduire au minimum les

valeurs de blanc ainsi que les avantages et les inconvénients de chaque méthode sont décrits de manière

détaillée dans les articles correspondants. D’autres indications concernant l’assurance qualité et les

problèmes liés aux valeurs de blanc qui doivent être prises en compte sont indiquées à l’Article 10.

4.2 Prélèvement par adsorption suivie d’une désorption thermique

Utiliser l’appareillage, les réactifs et les matériaux décrits dans l’ISO 16000-6 (y compris l’annexe

informative concernant les composés semi-volatils) avec les exigences spécifiques supplémentaires

suivantes:
4.2.1 Appareillage, matériaux et produits chimiques

4.2.1.1 Tube de désorption thermique, tube en acier inoxydable, en acier revêtu d’un matériau inerte,

ou en verre contenant une couche peu compacte de 1 cm de laine de quartz non friable additionnée d’au

moins 200 mg d’adsorbant, par exemple Tenax® TA 20/35 (voir l’ISO 16000-6:2011, Annexe D).

4.2.1.2 Système de prélèvement, selon la Figure 1.

4.2.1.3 Pompe, adaptée à un débit-volume compris entre 50 ml/min et 200 ml/min dans les conditions

de prélèvement; volume de prélèvement recommandé d’environ 20 l à environ 70 l.

4.2.1.4 Compteur volumétrique de gaz, dont l’incertitude de mesure maximale ne doit pas

dépasser 5 %.

4.2.1.5 Installations de prélèvement en laboratoire, hygromètre, thermomètre, baromètre.

1) Tenax® TA est l’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 signifie nullement que l’ISO approuve

ou recommande l’emploi exclusif du produit ainsi désigné. Des produits équivalents peuvent être utilisés s’il peut

être démontré qu’ils conduisent aux mêmes résultats.

2) Florisil® est l’appellation commerciale d’un produit fourni par U.S. Silica. Cette information est donnée, par

souci de commodité, à l’intention des utilisateurs du présent document et ne signifie nullement que l’ISO approuve

ou recommande l’emploi exclusif du produit ainsi désigné. Des produits équivalents peuvent être utilisés s’il peut

être démontré qu’ils conduisent aux mêmes résultats.
2 © ISO 2017 – Tous droits réservés
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ISO 16000-33:2017(F)

4.2.1.6 Étalons internes, requis comme mesure de contrôle de la qualité de l’ensemble du processus

d’analyse, y compris le prélèvement; les exemples appropriés comprennent: les composés cycliques

deutérés D4-DMP, D4-DEP, D4-DBP, D4-BBP, D4-DEHP, D4-DOP ainsi que le phtalate de diallyle non

deutéré (DAlP), voir Article 5 et Tableau 3. Les étalons doivent être préparés dans du méthanol exempt de

phtalate, comme décrit dans l’ISO 16000-6, à un niveau tel qu’une injection de 1 µl maximum introduise

environ la même masse d’analyte sur l’extrémité de prélèvement des tubes que celle qui est prévue d’être

collectée pendant le prélèvement.

4.2.1.7 Unité de désorption thermique, couplée à CPG-SM pour la désorption thermique en deux

étapes des tubes à sorbant et le transfert des vapeurs désorbées via un flux de gaz inerte dans un système

de chromatographie en phase gazeuse (CPG), équipé d’un détecteur à spectrométrie de masse (SM).

NOTE De la laine de verre désactivée (silanisée) ou de la laine de quartz peut également être utilisée comme

adsorbant après une validation appropriée de la méthode.
4.2.2 Préparation du tube de désorption thermique

L’utilisation d’un tube contenant une couche de laine de quartz additionnée de Tenax® TA suppose de

connaître la norme ISO 16000-6. Des tubes à sorbant préremplis et préconditionnés sont disponibles

dans le commerce ou peuvent être préparés au laboratoire comme suit:

Une couche de laine de quartz non friable, généralement supportée par une grille en acier inoxydable,

est insérée au niveau de l’extrémité de prélèvement du tube. La masse de sorbant requise est versée

dans le tube après la couche de laine de quartz. L’extrémité la plus éloignée de la couche de sorbant est

généralement supportée par une deuxième couche de laine de quartz ou une grille en acier inoxydable.

Au moins 200 mg de sorbant doivent être utilisés par tube afin de garantir la capacité de sorption.

NOTE La détermination du volume de claquage est décrite dans l’ISO 16017-1:2000, Annexe B. Les volumes

de claquage sont proportionnels aux dimensions et masses des sorbants. La règle empirique est que le volume

d’échantillon garanti double lorsque la longueur de la couche de sorbant est doublée (en conservant le même

diamètre de tube).

Après le remplissage des tubes de désorption thermique (par exemple avec du Tenax® TA ), les tubes

sont conditionnés pendant environ 8 h à 280 °C, puis pendant environ 30 min à 300 °C dans un flux

de gaz inerte (100 ml/min). Les tubes de sorption purifiés sont fermés et conservés à température

ambiante et à l’abri de la lumière dans un récipient empêchant la contamination des échantillons.

Analyser un nombre représentatif de tubes conditionnés pour déterminer une valeur à blanc à l’aide

de paramètres analytiques de routine, pour s’assurer que la valeur de blanc de désorption thermique

retenue est suffisamment faible (voir l’ISO 16000-6:2011, 7.1).

Il convient d’effectuer le prélèvement dès que possible après le conditionnement. Si le prélèvement ne

peut pas être réalisé dans un délai d’environ 14 jours après le conditionnement, le tube doit alors être

reconditionné pendant 15 min à environ 300 °C avant le prélèvement. Pour éviter toute contamination,

il convient de manipuler les tubes de désorption thermique uniquement avec des gants en coton. De

plus, l’étiquetage doit être omis.

Il convient que le système de thermodésorption ne permette aucun contact du flux d’échantillon avec

les surfaces externes des tubes. Si le système d’analyse choisi ne garantit pas cela, les tubes doivent être

manipulés uniquement avec des gants en coton propres, sur le terrain et au laboratoire, pour réduire

autant que possible la contamination.

Il convient d’identifier les tubes de manière individuelle et indélébile, mais sans apposer d’étiquette

adhésive susceptible de se défaire ou de se décolorer pendant la désorption thermique.

4.2.3 Prélèvement

Avant le prélèvement, les tubes conditionnés sont dopés avec au maximum 1 µl de solution d’étalon

interne dans du méthanol (par exemple 20 ng/µl pour un volume de prélèvement de 50 l; la masse

© ISO 2017 – Tous droits réservés 3
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ISO 16000-33:2017(F)

absolue d’étalon dopé ajouté dépend du volume de prélèvement et du domaine de mesure de la

méthode). La solution d’étalon est généralement introduite au niveau de l’extrémité de prélèvement du

tube à sorbant.

L’équipement de prélèvement est assemblé conformément à la Figure 1 et doit être exempt de fuites.

La pompe est raccordée à l’extrémité du tube ne servant pas au prélèvement, au moyen de raccords en

polyéthylène ou en polytétrafluoroéthylène (PTFE), et mise en marche. Si le volume de claquage des

phtalates analysés est inconnu, deux tubes de sorption doivent alors être raccordés en série. Les tubes

doivent être raccordés à l’aide d’un manchon exempt de phtalate.

Le débit-volume ainsi que la température, la pression atmosphérique absolue et l’humidité relative

de l’air doivent être enregistrés. Les débits-volumes de prélèvement appropriés sont compris entre

50 ml/min et 200 ml/min. Cela correspond à un volume de prélèvement recommandé d’environ 20 l à

70 l pour une durée de prélèvement d’environ 2 h à 24 h. Après le prélèvement, le tube de sorption est

retiré de l’équipement de prélèvement; les deux extrémités du tube de sorption doivent être obturées.

Un double prélèvement de l’air intérieur est recommandé.

Les tubes échantillonnés doivent être transportés au laboratoire et analysés dès que possible.

4.3 Prélèvement par adsorption suivie d’une extraction au solvant
4.3.1 Appareillage, matériels et produits chimiques
4.3.1.1 Système de prélèvement, selon la Figure 1.

4.3.1.2 Pompe, appropriée pour un débit-volume d’environ 2 l/min dans les conditions du

3 3
prélèvement; volume de prélèvement recommandé d’environ 1 m à 3 m en 8 h à 24 h.

4.3.1.3 Compteur volumétrique de gaz, dont l’incertitude de mesure maximale ne doit pas

dépasser 5 %.
4.3.1.4 Four à moufle.

4.3.1.5 Capsule d’évaporation plate, résistant à la chaleur, pour chauffer le Florisil® .

4.3.1.6 Florisil® , 60 à 100 mesh.
4.3.1.7 Laine de verre, silanisée.

4.3.1.8 Flacon en verre, muni d’un bouchon vissé et d’un joint en polytétrafluoroéthylène (PTFE), 50 ml.

4.3.1.9 Tubes d’adsorption, tube en verre, d’environ 200 mm de longueur et 10 mm à 12 mm de

diamètre intérieur.

4.3.1.10 Installations de prélèvement en laboratoire, hygromètre, thermomètre, baromètre.

4.3.1.11 Solvant, par exemple éther méthyl tert-butylique (TBME) ou toluène, sans valeurs de blanc (le

solvant doit être soumis à essai pour déterminer l’absence de valeurs de blanc de phtalates).

4.3.1.12 Étalons internes, Les étalons appropriés sont, par exemple, les composés cycliques deutérés

D4-DMP, D4-DEP, D4-DBP, D4-BBP, D4-DEHP, D4-DOP ainsi que le phtalate de diallyle non deutéré (DAlP);

voir Article 5 et Tableau 3.
4 © ISO 2017 – Tous droits réservés
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ISO 16000-33:2017(F)

4.3.1.13 CPG-SM, système de chromatographie en phase gazeuse (CPG), équipé d’un détecteur à

spectrométrie de masse (SM).
Légende
1 tube de prélèvement
2 pompe à vide à membrane
3 interrupteur à minuterie (facultatif)
4 filtre anti-abrasion
5 dispositif de mesure du volume ou régulateur de débit massique
6 boîtier de protection
Figure 1 — Représentation schématique de l’équipement de prélèvement
Légende
1 Florisil®
2 laine de verre
Figure 2 — Remplissage du tube en verre
4.3.2 Préparation du Florisil® et des tubes d’adsorption

Le Florisil® est étalé en une couche mince (d’environ 3 cm à 4 cm) sur une capsule d’évaporation et

chauffé à 800 °C pendant 6 h. Après refroidissement dans le dessiccateur, il est désactivé à l’aide d’eau

bi-distillée (proportion de 3 % en masse). À cet effet, 5 g de Florisil® et 150 µl d’eau sont introduits

dans un flacon en verre de 50 ml muni d’un bouchon vissé et d’un joint en polytétrafluoroéthylène

(PTFE). Après avoir fermé le flacon, le Florisil® doit être mélangé pendant environ 45 min jusqu’à

l’obtention d’une poudre s’écoulant uniformément. Le Florisil® désactivé est ensuite introduit dans

un tube d’adsorption (voir Figure 2). Il convient que la hauteur de remplissage soit d’environ 10 cm à

© ISO 2017 – Tous droits réservés 5
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ISO 16000-33:2017(F)
13 cm. Les extrémités de la couche de Florisil® sont obturées à l
...

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