SIST EN ISO 16017-1:2002

Indoor, ambient and workplace air - Sampling and analysis of volatile organic compounds by sorbent tube/thermal desorption/capillary gas chromatography - Part 1: Pumped sampling (ISO 16017-1:2000)

This part of ISO 16017 gives general guidance for the sampling and analysis of volatile organic compounds (VOCs)
in air. It is applicable to ambient, indoor and workplace atmospheres and the assessment of emissions from
materials in small- or full-scale test chambers.
This part of ISO 16017 is appropriate for a wide range of VOCs, including hydrocarbons, halogenated hydrocarbons,
esters, glycol ethers, ketones and alcohols. A number of sorbents 1) are recommended for the sampling of
these VOCs, each sorbent having a different range of applicability. Very polar compounds will generally require
derivatization, very low boiling compounds will only be partially retained by the sorbents, depending on ambient
temperature, and can only be estimated qualitatively. Semi-volatile compounds will be fully retained by the
sorbents, but may only be partially recovered. Compounds for which this part of ISO 16017 has been tested are
given in tables. This part of ISO 16017 may be applicable to compounds not listed, but in these cases it is
advisable to use a back-up tube containing the same or a stronger sorbent.
This part of ISO 16017 is applicable to the measurement of airborne vapours of VOCs in a concentration range of
approximately 0,5 _g/ m3 to 100 mg/m3 individual compound.
The upper limit of the useful range is set by the sorptive capacity of the sorbent used and by the linear dynamic
range of the gas chromatograph column and detector or by the sample-splitting capability of the analytical
instrumentation used. The sorptive capacity is measured as a breakthrough volume of air, which determines the
maximum air volume that shall not be exceeded when sampling.
The lower limit of the useful range depends on the noise level of the detector and on blank levels of analyte and/or
interfering artefacts on the sorbent tubes. Artefacts are typically sub-nanogram for well-conditioned Tenax GR and
carbonaceous sorbents such as Carbopack/Carbotrap type materials, carbonized molecular sieves and molecular
sieves such as Spherocarb, or pure charcoal; at low nanogram levels for Tenax TA and at 5 ng to 50 ng levels for
other porous polymers such as Chromosorbs and Porapaks. Sensitivity is typically limited to 0,5 _g/m_ for 10-litre
air samples with this latter group of sorbents because of their inherent high background.
The procedure specified in this part of ISO 16017 is applicable to low flowrate personal sampling pumps and gives
a time-weighted average result. It is not applicable to the measurement of instantaneous or short-term fluctuations
in concentration.
1) The sorbents listed in annex C and elsewhere in this International Standard are those known to perform as specified under
this part of ISO 16017. Each sorbent or product that is identified by a trademarked name is unique and has a sole manufacturer;
however, they are widely available from many different suppliers. This information is given for the convenience of users of this
part of ISO 16017 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.

Innenraumluft, Außenluft und Luft am Arbeitsplatz - Probenahme und Analyse flüchtiger organischer Verbindungen durch Sorptionsröhrchen/thermische Desorption/Kapillar-Gaschromatographie - Teil 1: Probenahme mit einer Pumpe (ISO 16017-1:2000)

Dieser Teil der ISO 16017 gibt allgemeine Hinweise für die Probenahme und Analyse flüchtiger organischer Verbindungen (VOC) in der Luft. Die Internationale Norm ist anwendbar für Außenluft, Innenraumluft und Luft am Arbeitsplatz und für die Bewertung von Emissionen aus Materialien in kleinen Prüfkammern oder Prüfräumen. Diese Internationale Norm ist für eine große Bandbreite von VOC, einschließlich Kohlenwasserstoffen, halogenierten Kohlen-wasserstoffen, Estern, Glykolethern, Ketonen und Alkoholen, anwendbar. Eine Vielzahl an Sorbenzien 1 ) wird für die Probe-nahme dieser VOC empfohlen; jedes Sorbenz hat einen unterschiedlichen Anwendungsbereich. Sehr polare Verbindungen er-fordern im allgemeinen eine Derivatisierung. Verbindungen mit sehr niedrigem Siedepunkt werden - in Abhängigkeit von den Außentemperaturen - nur partiell von den Sorbenzien zurückgehalten und können nur qualitativ abgeschätzt werden. Semi-flüchtige Verbindungen werden vollständig durch die Sorbenzien zurückgehalten, können aber nur zum Teil wiedergefunden werden. Die Verbindungen, die im Rahmen dieses Teils der ISO 16017 geprüft wurden, sind in den Tabellen aufgeführt. Die Interna-tionale Norm kann auch zur Bestimmung nicht aufgeführter Verbindungen angewendet werden; in diesen Fällen ist es aber rat-sam, ein Sicherheitsröhrchen am Ende der Probenahmeapparatur mit dem gleichen oder einem stärkeren Sorbenz zu ver-wenden.
Dieser Teil der ISO 16017 ist anwendbar für die Messung von luftgetragenen VOC-haltigen Dämpfen im Konzentrations-bereich
von ungefähr 0,5 microg/m - bis 100 mg/m 3 für jede einzelne Verbindung. Die obere Nachweisgrenze eines sinnvollen Anwendungsbereiches wird durch die Sorptionskapazität des verwendeten Sorbenz und durch den linearen dynamischen Bereich der Gaschromatographiesäule und des Detektors oder durch die Beschaffenheit des Probensplits in dem verwendeten analytischen Gerät festgelegt...(Abgeschnitten)

Air intérieur, air ambiant et air des lieux de travail -Echantillonnage et analyse des composés organiques volatils par tube a adsorption/désorption thermique/chromatographie en phase gazeuse sur capillaire - Partie 1: Echantillonnage par pompage (ISO 16017-1:2000)

La présente partie de l'ISO 16017 donne des lignes directrices générales portant sur l'échantillonnage et l'analyse
des composés organiques volatils (COV) dans l'air. Elle est applicable aux atmosphères ambiantes, à l'intérieur
des bâtiments et sur les lieux de travail, ainsi qu'à l'évaluation des émissions par des matériaux dans des
chambres d'essai de petite taille ou en grandeur réelle.
La présente partie de l'ISO 16017 convient à un grand nombre de COV, y compris les hydrocarbures, les
hydrocarbures halogénés, les esters, les éthers de glycol, les cétones et les alcools. Certains adsorbants1) sont
recommandés pour l'échantillonnage de ces COV, chaque adsorbant ayant des applications particulières. Les
composés fortement polaires doivent généralement être dérivés; les composés à point d'ébullition très bas sont
seulement partiellement retenus par les adsorbants, selon la température ambiante, et leur évaluation ne peut être
que qualitative. En revanche, les composés semi-volatils sont totalement retenus par les adsorbants mais ne
peuvent être que partiellement récupérables. Les composés pour lesquels la présente partie de l'ISO 16017 a fait
l'objet d'essais sont indiqués dans les tableaux. La présente partie de l'ISO 16017 peut s'appliquer à des
composés non cités, mais dans ce cas il est conseillé de prévoir un tube avec une deuxième plage contenant le
même adsorbant, ou un adsorbant plus puissant.
La présente partie de l'ISO 16017 est applicable au mesurage des vapeurs de COV en suspension dans l'air dans
une étendue de concentrations des composés organiques individuels comprise entre 0,5 μg/m3 et 100 mg/m3
environ.
La limite supérieure de l'étendue utile est déterminée par la capacité d'adsorption de l'adsorbant utilisé et par
l'étendue dynamique linéaire de la colonne et du détecteur du chromatographe en phase gazeuse ou par la
capacité de séparation des échantillons des instruments d'analyse utilisés. La capacité d'adsorption est mesurée
sous forme d'un volume de claquage de l'air qui détermine le volume d'air maximal ne devant pas être dépassé
lors de l'échantillonnage.
La limite inférieure de l'étendue utile dépend du niveau de bruit du détecteur et des niveaux à blanc de l'analyte
et/ou des artefacts d'interférences sur les tubes à adsorption. Ces artefacts sont généralement d'un ordre inférieur
au nanogramme pour les Tenax GR et les adsorbants carbonés tels que les matériaux de type
Carbopack/Carbotrap, les tamis moléculaires au carbone et les tamis moléculaires tels que le Spherocarb, ou le
charbon pur; ils correspondent à de faibles niveaux de l'ordre du nanogramme pour le Tenax TA et au niveau situé
1) Les adsorbants cités à l'annexe C et ailleurs dans la présente partie de l'ISO 16017 sont ceux qui ont un comportement
connu pour être conforme à la présente partie de l'ISO 16017. Chaque adsorbant ou produit identifié par un nom de marque
commerciale est unique et est produit par un seul fabricant; il peut cependant être disponible auprès de plusieurs fournisseurs.
Cette information est donnée à l'intention des utilisateurs de la présente partie de l'ISO 16017 et ne signifie nullement que l'ISO
approuve ou recommande l'emploi exclusif des produits ainsi désignés. Des produits équivalents peuvent être utilisés s'il est
démontré qu'ils conduisent aux mêmes résultats.
entre 5 ng et 50 ng pour les autres polymères poreux tels que les Chromosorbs et les Porapaks. La sensibilité est
généralement limitée à 0,5 μg/m3 pour des écha

Notranji in zunanji zrak ter zrak na delovnem mestu - Vzorčenje in analiza hlapnih organskih spojin z absorpcijskimi cevkami in kapilarno plinsko kromatografijo s toplotno desorpcijo - 1. del: Vzorčenje s črpanjem (ISO 16017–1.2000)

General Information

• Status: Published
• Publication Date: 30-Apr-2002
• ICS: 13.040.01 - Air quality in general
• Technical Committee: KAZ - Air quality
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 01-May-2002
• Due Date: 01-May-2002
• Completion Date: 01-May-2002
• Ref Project: EN ISO 16017-1:2000 - Indoor, ambient and workplace air - Sampling and analysis of volatile organic compounds by sorbent tube/thermal desorption/capillary gas chromatography - Part 1: Pumped sampling (ISO 16017-1:2000)

Standards Content (Sample)

SLOVENSKI STANDARD
SIST EN ISO 16017-1:2002
01-maj-2002
1RWUDQMLLQ]XQDQML]UDNWHU]UDNQDGHORYQHPPHVWX9]RUþHQMHLQDQDOL]DKODSQLK
RUJDQVNLKVSRMLQ]DEVRUSFLMVNLPLFHYNDPLLQNDSLODUQRSOLQVNRNURPDWRJUDILMRV
WRSORWQRGHVRUSFLMRGHO9]RUþHQMHVþUSDQMHP,62±
Indoor, ambient and workplace air - Sampling and analysis of volatile organic
compounds by sorbent tube/thermal desorption/capillary gas chromatography - Part 1:
Pumped sampling (ISO 16017-1:2000)
Innenraumluft, Außenluft und Luft am Arbeitsplatz - Probenahme und Analyse flüchtiger
organischer Verbindungen durch Sorptionsröhrchen/thermische Desorption/Kapillar-
Gaschromatographie - Teil 1: Probenahme mit einer Pumpe

(ISO 16017-1:2000)
Air intérieur, air ambiant et air des lieux de travail -Echantillonnage et analyse des
composés organiques volatils par tube a adsorption/désorption
thermique/chromatographie en

phase gazeuse sur capillaire - Partie 1: Echantillonnage par pompage (ISO 16017-
1:2000)
Ta slovenski standard je istoveten z: EN ISO 16017-1:2000
ICS:
13.040.01 Kakovost zraka na splošno Air quality in general
SIST EN ISO 16017-1:2002 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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INTERNATIONAL ISO
STANDARD 16017-1
First edition
2000-11-15
Indoor, ambient and workplace air —
Sampling and analysis of volatile organic
compounds by sorbent tube/thermal
desorption/capillary gas
chromatography —
Part 1:
Pumped sampling
Air intérieur, air ambiant et air des lieux de travail — Échantillonnage et
analyse des composés organiques volatils par tube à
adsorption/désorption thermique/chromatographie en phase gazeuse sur
capillaire —
Partie 1: Échantillonnage par pompage
Reference number
ISO 16017-1:2000(E)
©
ISO 2000

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ISO 16017-1:2000(E)
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ii © ISO 2000 – All rights reserved

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ISO 16017-1:2000(E)
Contents Page
Foreword.iv
1 Scope .1
2 Normative references .2
3 Terms and definitions .2
4 Principle.3
5 Reagents and materials .3
6 Apparatus .5
7 Sample tube conditioning.6
8 Calibration of pump.7
9 Sampling.7
10 Procedure .8
10.1 Safety precautions.8
10.2 Desorption and analysis .8
10.3 Calibration .9
10.4 Determination of sample concentration.10
10.5 Determination of desorption efficiency.10
11 Calculations.10
11.1 Mass concentration of analyte .10
11.2 Volume concentration of analyte .11
12 Interferences .11
13 Performance characteristics .11
14 Test report .12
15 Quality control.12
Annex A (normative) Determination of breakthrough volumes from gas standards.21
Annex B (normative) Determination of breakthrough volume from the extrapolated retention volume.22
Annex C (informative) Description of sorbent types .23
Annex D (informative) Guidance on sorbent selection .24
Annex E (informative) Guidance on sorbent use .25
Annex F (informative) Summary of data on overall uncertainty, precision, bias and storage.26
Bibliography.28
© ISO 2000 – All rights reserved iii

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ISO 16017-1:2000(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.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3.
Draft International Standards adopted by the technical committees are circulated to the member bodies for voting.
Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this part of ISO 16017 may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights.
International Standard ISO 16017-1 was prepared by Technical Committee ISO/TC 146, Air quality, Subcommittee
SC 6, Indoor air.
ISO 16017 consists of the following parts, under the general title Indoor, ambient and workplace air — Sampling
and analysis of volatile organic compounds by sorbent tube/thermal desorption/capillary gas chromatography:
� Part 1: Pumped sampling
� Part 2: Diffusive sampling
Annexes A and B form a normative part of this part of ISO 16017. Annexes C through F are for information only.
iv © ISO 2000 – All rights reserved

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INTERNATIONAL STANDARD ISO 16017-1:2000(E)
Indoor, ambient and workplace air — Sampling and analysis of
volatile organic compounds by sorbent tube/thermal
desorption/capillary gas chromatography —
Part 1:
Pumped sampling
1 Scope
This part of ISO 16017 gives general guidance for the sampling and analysis of volatile organic compounds (VOCs)
in air. It is applicable to ambient, indoor and workplace atmospheres and the assessment of emissions from
materials in small- or full-scale test chambers.
This part of ISO 16017 is appropriate for a wide range of VOCs, including hydrocarbons, halogenated hydro-
1)
carbons, esters, glycol ethers, ketones and alcohols. A number of sorbents are recommended for the sampling of
these VOCs, each sorbent having a different range of applicability. Very polar compounds will generally require
derivatization, very low boiling compounds will only be partially retained by the sorbents, depending on ambient
temperature, and can only be estimated qualitatively. Semi-volatile compounds will be fully retained by the
sorbents, but may only be partially recovered. Compounds for which this part of ISO 16017 has been tested are
given in tables. This part of ISO 16017 may be applicable to compounds not listed, but in these cases it is
advisable to use a back-up tube containing the same or a stronger sorbent.
This part of ISO 16017 is applicable to the measurement of airborne vapours of VOCs in a concentration range of
3 3
approximately 0,5�g/ m to 100 mg/m individual compound.
The upper limit of the useful range is set by the sorptive capacity of the sorbent used and by the linear dynamic
range of the gas chromatograph column and detector or by the sample-splitting capability of the analytical
instrumentation used. The sorptive capacity is measured as a breakthrough volume of air, which determines the
maximum air volume that shall not be exceeded when sampling.
The lower limit of the useful range depends on the noise level of the detector and on blank levels of analyte and/or
interfering artefacts on the sorbent tubes. Artefacts are typically sub-nanogram for well-conditioned Tenax GR and
carbonaceous sorbents such as Carbopack/Carbotrap type materials, carbonized molecular sieves and molecular
sieves such as Spherocarb, or pure charcoal; at low nanogram levels for Tenax TA and at 5 ng to 50 ng levels for
�
other porous polymers such as Chromosorbs and Porapaks. Sensitivity is typically limited to 0,5 �g/m for 10-litre
air samples with this latter group of sorbents because of their inherent high background.
The procedure specified in this part of ISO 16017 is applicable to low flowrate personal sampling pumps and gives
a time-weighted average result. It is not applicable to the measurement of instantaneous or short-term fluctuations
in concentration.
1) The sorbents listed in annex C and elsewhere in this International Standard are those known to perform as specified under
this part of ISO 16017. Each sorbent or product that is identified by a trademarked name is unique and has a sole manufacturer;
however, they are widely available from many different suppliers. This information is given for the convenience of users of this
part of ISO 16017 and does not constitute an endorsement by ISO of the product named. Equivalent products may be used if
they can be shown to lead to the same results.
© ISO 2000 – All rights reserved 1

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ISO 16017-1:2000(E)
2 Normative references
The following normative documents contain provisions which, through reference in this text, constitute provisions of
this part of ISO 16017. For dated references, subsequent amendments to, or revisions of, any of these publications
do not apply. However, parties to agreements based on this part of ISO 16017 are encouraged to investigate the
possibility of applying the most recent editions of the normative documents indicated below. For undated
references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain
registers of currently valid International Standards.
ISO 5725-1:1994, Accuracy (trueness and precision) of measurement methods and results — Part 1: General
principles and definitions.
ISO 5725-2:1994, Accuracy (trueness and precision) of measurement methods and results — Part 2: Basic method
for the determination of repeatability and reproducibility of a standard measurement method.
ISO 6141:2000, Gas analysis — Requirements for certificates for calibration gases and gas mixtures.
ISO 6145-1:1986, Gas analysis — Preparation of calibration gas mixtures using dynamic volumetric methods —
Part 1: Methods of calibration.
ISO 6145-3:1986, Gas analysis — Preparation of calibration gas mixtures — Dynamic volumetric methods —
Part 3: Periodic injections into a flowing gas stream.
ISO 6145-4:1986, Gas analysis — Preparation of calibration gas mixtures — Dynamic volumetric methods —
Part 4: Continuous injection method.
2)
ISO 6145-5:— , Gas analysis — Preparation of calibration gas mixtures using dynamic volumetric methods —
Part 5: Capillary calibration devices.
2)
ISO 6145-6:— , Gas analysis — Preparation of calibration gas mixtures using dynamic volumetric methods —
Part 6: Critical orifices.
ISO 6349:1979, Gas analysis — Preparation of calibration gas mixtures — Permeation method.
EN 1076:1997, Workplace atmospheres — Pumped sorbent tubes for the determination of gases and vapours —
Requirements and test methods.
3 Terms and definitions
For the purposes of this part of ISO 16017, the following terms and definitions apply.
3.1
breakthrough volume
volume of test atmosphere that can be passed through a sorbent tube before the concentration of eluting vapour
reaches 5 % of the applied test concentration
NOTE 1 The breakthrough volume varies with the vapour and the sorbent type.
NOTE 2 See reference [4]. 3.2
retention volume
elution volume at peak maximum of a small aliquot of an organic vapour eluted from a sorbent tube by air or
chromatographic carrier gas
2) To be published.
2 © ISO 2000 – All rights reserved

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ISO 16017-1:2000(E)
4Principle
A measured volume of sample air is drawn through one (or more) sorbent tubes in series; an appropriate sorbent
(or sorbents) being selected for the compound or mixture to be sampled. Provided suitable sorbents are chosen,
volatile organic components are retained by the sorbent tube and thus are removed from the flowing air stream.
The collected vapour (on each tube) is desorbed by heat and is transferred under inert carrier gas into a gas
chromatograph equipped with a capillary column and a flame ionization detector or other suitable detector, where it
is analysed. Analytical calibration is achieved by means of liquid or vapour spiking onto a sorbent tube.
5 Reagents and materials
During the analysis, use only reagents of recognized analytical reagent grade.
Fresh standard calibration blend solutions should be prepared weekly, or more frequently if evidence is noted of
deterioration, e.g. condensation reactions between alcohols and ketones.
5.1 Volatile organic compounds, for calibration purposes, using either liquid spiking (5.7 and 5.8) or vapour
spiking (5.4 to 5.6) onto sorbent tubes.
5.2 Dilution solvent, for preparing calibration blend solution for liquid spiking (5.7). This should be of
chromatographic quality. It shall be free from compounds co-eluting with the compound or compounds of interest
(5.1).
NOTE Methanol is frequently used. Alternative dilution solvents e.g. ethyl acetate or cyclohexane, can be used, particularly
if there is no possibility of reaction or chromatographic co-elution.
5.3 Sorbents, of recommended particle size 0,18 mm to 0,25 mm (60 to 80 mesh).
Each sorbent should be preconditioned under a flow of inert gas by heating it overnight (= 16 h) at a temperature at
least 25�C below the published maximum for that sorbent before packing the tubes. To prevent recontamination of
the sorbents, they shall be kept in a clean atmosphere during cooling to room temperature, storage, and loading
into the tubes. Wherever possible, analytical desorption temperatures should be kept below those used for
conditioning. Tubes prepacked by the manufacturer are also available for most sorbents and as such only require
conditioning.
NOTE 1 Sorbent particle sizes larger than 0,18 mm to 0,25 mm may be used but the breakthrough characteristics given in
Tables 1 to 6 may be affected. Smaller sorbent particle size ranges are not recommended because of back-pressure problems.
NOTE 2 A description of sorbents is given in annex C and a guide for sorbent selection is given in annex D. Equivalent
sorbents may be used. A guide to sorbent conditioning and analytical desorption parameters is given in annex E.
5.4 Calibration standards, preferably prepared by loading required amounts of the compounds of interest on
sorbent tubes from standard atmospheres (see 5.5 and 5.6), as this procedure most closely resembles the practical
sampling situation.
If this way of preparation is not practicable, standards may be prepared by a liquid spiking procedure (see 5.7 and
5.8), provided that the accuracy of the spiking technique is either:
a) established by using procedures giving spiking levels fully traceable to primary standards of mass and/or
volume, or,
b) confirmed by comparison with reference materials, if available, standards produced using standard
atmospheres, or results of reference measurement procedures.
NOTE The loading ranges given in 5.6, 5.7 and 5.8 are not mandatory and approximate to the application range given in
clause 1 for a 2-litre sample. For specific applications in which larger volumes are used to measure lower concentrations, other
loading ranges may be more appropriate.
© ISO 2000 – All rights reserved 3

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ISO 16017-1:2000(E)
5.5 Standard atmospheres.
Prepare standard atmospheres of known concentrations of the compound(s) of interest by a recognized procedure.
Methods described in ISO 6141, the appropriate part of ISO 6145 and ISO 6349 are suitable. If the procedure is
not applied under conditions that allow the establishment of full traceability of the generated concentrations to
primary standards of mass and/or volume, or if the chemical inertness of the generation system cannot be
guaranteed, the concentrations shall be confirmed using an independent procedure.
5.6 Standard sorbent tubes, loaded by spiking from standard atmospheres.
Prepare loaded sorbent tubes by passing an accurately known volume of the calibration atmosphere through the
sorbent tube, e.g. by means of a pump. The volume of atmosphere sampled shall not exceed the breakthrough
volume of the analyte sorbent combination. After loading, disconnect and seal the tube. Prepare fresh standards
3 3
with each batch of samples. Prepare standard atmospheres equivalent to 10 mg/m and 100�g/m . For workplace
3
air, load sorbent tubes with 100 ml, 200 ml, 400 ml, 1 l, 2 l, or 4 l of the 10 mg/m atmosphere. For ambient or
3
indoor air, load sorbent tubes with 100 ml, 200 ml, 400 ml, 1 l, 2 l, 4 l or 10 l of the 100�g/m atmosphere.
5.7 Solutions for liquid spiking.
5.7.1 Solution containing approximately 10 mg/ml of each liquid component.
Accurately weigh approximately 1 g of substance or substances of interest into a 100 ml volumetric flask, starting
with the least volatile substance. Make up to 100 ml with dilution solvent (5.2), stopper and shake to mix.
5.7.2 Solution containing approximately 1 mg/ml of liquid components.
Introduce 50 ml of dilution solvent into a 100 ml volumetric flask. Add 10 ml of solution 5.7.1 Make up to 100 ml with
dilution solvent, stopper and shake to mix.
5.7.3 Solution containing approximately 100 ����g/ml of each liquid component.
Accurately weigh approximately 10 mg of substance or substances of interest into a 100 ml volumetric flask,
starting with the least volatile substance. Make up to 100 ml with dilution solvent (5.2), stopper and shake to mix.
5.7.4 Solution containing approximately 10 ��g/ml of liquid components.
��
Introduce 50 ml of dilution solvent into a 100 ml volumetric flask. Add 10 ml of solution described in 5.7.3. Make up
to 100 ml with dilution solvent, stopper and shake to mix.
5.7.5 Solution containing approximately 1 mg/ml of gas components.
For gases, e.g. ethylene oxide, a high level calibration solution may be prepared as follows. Obtain gas at
atmospheric pressure by filling a small plastic gas bag from a gas cylinder containing pure gas. Fill a 1-ml gas-tight
syringe with 1 ml of the pure gas and close the valve of the syringe. Using a 2-ml septum vial, add 2 ml dilution
solvent and close with the septum cap. Insert the tip of the syringe needle through the septum cap into the dilution
solvent. Open the valve and withdraw the plunger slightly to allow the dilution solvent to enter the syringe. The
action of the gas dissolving in the dilution solvent creates a vacuum, and the syringe fills with solvent. Return the
solution to the flask. Flush the syringe twice with the solution and return the washings to the flask. Calculate the
mass of gas added using the gas laws, i.e. 1 mole of gas at STP (standard temperature and pressure: 273,15 K
and 1 013,25 hPa) occupies 22,4 litres, but correct for any non-ideality of the particular pure gas compound.
4 © ISO 2000 – All rights reserved

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ISO 16017-1:2000(E)
5.7.6 Solution containing approximately 10µg/ml of gas components.
For gases, e.g. ethylene oxide, a low-level calibration solution may be prepared as follows. Obtain pure gas at
atmospheric pressure by filling a small plastic gas bag from a gas cylinder. Fill a 10-µl gas-tight syringe with 10µl
of the pure gas and close the valve of the syringe. Using a 2-ml septum vial, add 2 ml dilution solvent and close
with the septum cap. Insert the tip of the syringe needle through the septum cap into the dilution solvent. Open the
valve and withdraw the plunger slightly to allow the dilution solvent to enter the syringe. The action of the gas
dissolving in the dilution solvent creates a vacuum, and the syringe fills with solvent. Return the solution to the
flask. Flush the syringe twice with the solution and return the washings to the flask. Calculate the mass of gas
added using the gas laws, i.e. 1 mole of gas at STP occupies 22,4 litres, but correct for any non-ideality of the
particular pure gas compound.
5.8 Standard sorbent tubes loaded by liquid spiking.
Prepare loaded sorbent tubes by injecting aliquots of standard solutions onto clean sorbent tubes as follows. Fit a
sorbent tube into the injection unit (6.10) through which inert purge gas and a 1µl to 4µl aliquot of an appropriate
standard solution, injected through the septum, are passed. After an appropriate time, disconnect and seal the
tube. Prepare fresh standards with each batch of samples. For workplace air, load sorbent tubes with 1µl to 5µl of
solutions 5.7.1, 5.7.2 or 5.7.5. For ambient and indoor air, load sorbent tubes with 1µl to 5µl of solutions 5.7.3,
5.7.4 or 5.7.6.
NOTE In the case of methanol, a purge gas flowrate of 100 ml/min and a 5 min purge time have been found to be
appropriate to eliminate most of the solution solvent from the tube. If other dilution solvents are used, the conditions should be
determined experimentally.
6 Apparatus
Use ordinary laboratory apparatus and the following.
6.1 Sorbent tubes, compatible with the thermal desorption apparatus to be used (6.9).
Typically, but not exclusively, sorbent tubes are constructed of stainless steel tubing, 6,3 mm (1/4 inch) OD, 5 mm
ID and 90 mm long. Tubes of other dimensions may be used but the safe sampling volumes (SSV) given in
Tables 1 to 6 are based on these tube dimensions. For labile analytes, such as sulfur-containing compounds,
glass-lined or glass tubes (typically 4 mm ID) should be used. One end of the tube is marked, for example by a
scored ring about 10 mm from the sampling inlet end. The tubes are packed with one or more preconditioned
sorbents (5.3) so that the sorbent bed will be within the desorber heated zone and a gap of at least 14 mm is
retained at each end to minimize errors due to diffusive ingress at very low pump flowrates. Tubes contain between
200 mg and 1 000 mg sorbent, depending on sorbent density (typically about 250 mg porous polymer or 500 mg
carbon molecular sieve or graphitized carbon). The sorbents are retained by stainless steel gauzes and/or
unsilanized glass wool plugs. If more than one sorbent is used in a single tube, the sorbents should be arranged in
order of increasing sorbent strength and separated by unsilanized glass wool, with the weakest sorbent nearest to
the marked sampling inlet end of the tube.
Do not pack sorbents with widely different (� 50�C) maximum desorption temperatures into a single tube, or it will
be impossible to condition or desorb the more stable sorbent(s) sufficiently thoroughly without causing degradation
of the least stable sorbent(s).
6.2 Sorbent tube end caps.
The tubes shall be sealed according to the requirements of EN 1076:1997, subclause 5.6, or equivalent, e.g. with
metal screw-cap fittings with polytetrafluoroethylene (PTFE) seals.
6.3 Sorbent tube unions.
Two sorbent tubes may be connected in series during sampling with metal screw-cap couplings with PTFE seals.
© ISO 2000 – All rights reserved 5

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ISO 16017-1:2000(E)
6.4 Syringes, including a precision 10µl liquid syringe readable to 0,1µl, a precision 10 �l gas-tight syringe
readable to 0,1µl and a precision 1 ml gas-tight syringe readable to 0,01 ml.
6.5 Sampling pump
The pump should fulfil the requirements of EN 1232 [10] or equivalent.
The sampling pump shall be in accordance with local safety regulations.
6.6 Plastic or rubber tubing, about 90 cm long, of appropriate diameter to ensure a leak-proof fit to both pump
and sample tube or tube holder, if used. Clips should be provided to hold the sample tube and connecting tubing.
Sampling tubes shall not be used with plastic or rubber tubing upstream of the sorbent. The use of such tubing may
introduce contaminants or sorbed sampled VOCs.
6.7 Soap-bubble meter or other suitable device for calibrating pump.
The flow meter shall be traceably calibrated to a primary flow standard.
NOTE The use of an uncalibrated integral flow meter for the calibration of pump flowrates may result in systematic errors of
several tens of percent.
6.8 Gas chromatograph, fitted with a flame ionization, photoionization detector, mass spectrometric or other
suitable detector, capable of detecting an injection of 0,5 ng toluene with a signal-to-noise ratio of at least 5 to 1.
The gas chromatograph shall have a capillary column capable of separating the analytes of interest from other
components.
6.9 Thermal desorption apparatus, for the two-stage thermal desorption of the sorbent tubes and transfer of
the desorbed vapours via an inert gas flow into a gas chromatograph.
A typical apparatus contains a mechanism for holding the tubes to be desorbed whilst they are heated and purged
simultaneously with inert carrier gas. The desorption temperature and time is adjustable, as is the carrier gas
flowrate. The apparatus should also incorporate additional features, such as automatic sample tube loading, leak
testing, and a cold trap in the transfer line to concentrate the desorbed sample (10.2). The desorbed sample,
contained in the purge gas, is routed to the gas chromatograph and capillary column via a heated transfer line.
6.10 Injection facility for preparing standards by liquid spiking.
A conventional gas chromatographic injection port may be used for preparing sample tube standards. This can be
used in situ, or it can be mounted separately. The carrier gas line to the injector
...