Indoor air - Part 13: Determination of total (gas and particle-phase) polychlorinated dioxin-like biphenyls (PCBs) and polychlorinated dibenzo-p-dioxins/dibenzofurans (PCDDs/PCDFs) - Collection on sorbent-backed filters

This part of ISO 16000 specifies sampling and preparation of sampling media for dioxin-like polychlorinated biphenyls (PCBs), polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) in indoor air (see Table C.1). The method incorporates a sampling procedure that collects PCBs and PCDFs/PCDDs from air on a fine-particle filter backed up by a sorbent trap. The method cannot be used to separately determine gaseous PCBs and PCDFs/PCDDs and those that are particle-associated because some of the compounds will volatilize from the filter and be collected by the sorbent trap. This part of ISO 16000 does not address analytical methods for PCBs PCDDs and PCDFs, which are included in ISO 16000-14. (ISO 16000-13 and ISO 16000-14 are both parts of the overall measurement procedure for the determination of PCBs and PCDDs/PCDFs.) Combined with the analytical procedures specified in ISO 16000-14, which incorporate specific analyses by high-resolution gas chromatography combined with high-resolution mass spectrometry (HRGC/HRMS), this method is capable of detecting 0,2 pg/m3 or lower concentrations of most PCBs and PCDFs/PCDDs. However, it may not be possible to detect all analytes at 0,2 pg/m3 or lower, especially at lower sampling rates. To achieve adequate detection limits, no less than 50 m3 of air should be sampled. For normal measurement tasks, sampling volumes up to 360 m3 are employed (equivalent to a sampling period of 24 h at 16 m3/h or 7 d at 2 m3/h). The method has been validated for sampling periods up to seven days. With the use of larger sorbent traps, sampling volumes up to 1 000 m3 have been validated. Sampling precision under normal conditions can be expected to be 25 % or better and uncertainty 50 % or better. If the appropriate restrictions are applied, this method can be used for small rooms, for example children's rooms as well as for offices.

Air intérieur - Partie 13: Dosage des polychlorobiphényles (PCB) de type dioxine et des polychlorodibenzo-p-dioxines (PCDD)/polychlorodibenzofuranes (PCDF) totaux (en phase gazeuse et en phase particulaire) - Collecte sur des filtres adsorbants

L'ISO 16000‑13:2008 sp�cifie l'�chantillonnage et la pr�paration des supports d'�chantillonnage des polychlorobiph�nyles (PCB) de type dioxine, des polychlorodibenzo-p-dioxines (PCDD) et des polychlorodibenzofuranes (PCDF) dans l'air int�rieur. La m�thode int�gre un mode op�ratoire d'�chantillonnage dans lequel les PCB et les PCDD/PCDF sont pr�lev�s dans l'air sur un filtre � fines particules muni d'un pi�ge adsorbant. La m�thode ne convient pas au dosage s�par� des PCB et des PCDD/PCDF gazeux et de ceux li�s aux particules car certains compos�s qui s'�vaporent du filtre sont recueillis par le pi�ge adsorbant. L'ISO 16000‑13:2008 ne concerne pas les m�thodes analytiques relatives aux PCB, PCDD et PCDF qui sont trait�es dans l'ISO 16000‑14.

Notranji zrak - 13. del: Določevanje celotnih (v plinih in delcih) polikloriranih dioksinu podobnih bifenilov (PCB) in polikloriranih dibenzo-p-dioksinov/dibenzofuranov (PCDD/PCDF) - Zbiranje na filtrih z absorbentom

Ta del standarda ISO 16000 navaja vzorčenje in pripravo medija za vzorčenje dioksinom podobnih polikloriranih bifenilov (PCB), polikloriranih dibenzo-p-dioksinov (PCDD) in polikloriranih dibenzofluranov (PCDF) v notranjem zraku (glej preglednico C.1). Ta metoda vključuje postopek vzorčenja, s katerim se poliklorirani bifenili in poliklorirani dibenzo-p-dioksini/poliklorirani dibenzoflurani v zraku zbirajo na finem filtru, za katerim je absorbentna past. Te metode se ne more uporabiti za ločeno ugotavljanje plinastih polikloriranih bifenilov, polikloriranih dibenzo-p-dioksinov/polikloriranih dibenzofluranov in tistih spojin, ki so vezane na delce, ker bodo nekatere spojine izhlapele iz filtra in se bodo zbrale v absorbentni pasti. Ta del standarda ISO 16000 ne obravnava analiznih metod za poliklorirane bifenile, poliklorirane dibenzo-p-dioksine/poliklorirane dibenzoflurane, ki so vključeni v ISO 16000-14. ISO 16000-13 in ISO 16000-14 sta del celotnega meritvenega postopka za določevanje prisotnosti polikloriranih bifenilov, polikloriranih dibenzo-p-dioksinov/polikloriranih dibenzofluranov. Skupaj z analiznimi postopki, določenimi v standardu ISO 16000-14, ki vključuje posebne analize z visokoločljivostno plinsko kromatografijo v kombinaciji z visokoločljivostno masno spektrometrijo (HRGC/HRMS), je s to metodo mogoče zaznati koncentracije, enake ali nižje od 0,2 pg/m3, večine polikloriranih bifenilov, polikloriranih dibenzo-p-dioksinov/polikloriranih dibenzofluranov. Toda morda ni mogoče zaznati vseh analitov pri koncentraciji, enaki, ali nižji od 0,2 pg/m3, predvsem pri manjših količinah vzorcev. Za doseganje ustrezne meje zaznavnosti je potrebno vzorčiti vsaj 50 m3 zraka. Za običajne naloge vzorčenja se uporabi vzorce do 360 m3 (kar je enako vzorčenju v 24 urah pri 16 m3/h ali 7 dneh pri 2 m3/h). Ta metoda je bila validirana za obdobja vzorčenja do sedem dni. Z uporabo večjih absorbentnih pasti so bile validirane količine vzorcev do 1000 m3. Pod normalnimi pogoji se pričakuje, da bo natančnost vzorčenja 25 % ali več, negotovost pa 50 % ali boljša. Pri uporabi pravih omejitev se ta metoda lahko uporablja za majhne prostore, na primer otroške sobe in pisarne.

General Information

Status
Published
Public Enquiry End Date
31-May-2013
Publication Date
10-Nov-2013
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
08-Nov-2013
Due Date
13-Jan-2014
Completion Date
11-Nov-2013

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INTERNATIONAL ISO
STANDARD 16000-13
First edition
2008-11-01
Indoor air —
Part 13:
Determination of total (gas and particle-
phase) polychlorinated dioxin-like
biphenyls (PCBs) and polychlorinated
dibenzo-p-dioxins/dibenzofurans
(PCDDs/PCDFs) — Collection on sorbent-
backed filters
Air intérieur —
Partie 13: Dosage des polychlorobiphényles (PCB) de type dioxine et
des polychlorodibenzo-p-dioxines (PCDD)/polychlorodibenzofuranes
(PCDF) totaux (en phase gazeuse et en phase particulaire) — Collecte
sur des filtres adsorbants
Reference number
ISO 16000-13:2008(E)
ISO 2008
---------------------- Page: 1 ----------------------
ISO 16000-13:2008(E)
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ii © ISO 2008 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 16000-13:2008(E)
Contents Page

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

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

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

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

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

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

5 Principle..................................................................................................................................................4

6 Apparatus and materials.......................................................................................................................4

7 Preparation of sampling media............................................................................................................9

8 Sampling...............................................................................................................................................10

9 Minimum requirements for sampling ................................................................................................12

Annex A (informative) Details of samplers.....................................................................................................13

Annex B (normative) Determination of sampling efficiency or dynamic retention efficiency..................24

Annex C (informative) Structure, toxicity and calculation of toxicity equivalents.....................................25

Bibliography......................................................................................................................................................30

© ISO 2008 – All rights reserved iii
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ISO 16000-13:2008(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 2.

The main task of technical committees is to prepare International Standards. 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 document may be the subject of patent

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

ISO 16000-13 was prepared by Technical Committee ISO/TC 146, Air quality, Subcommittee SC 6, Indoor air.

ISO 16000 consists of the following parts, under the general title Indoor air:
⎯ Part 1: General aspects of sampling strategy
⎯ Part 2: Sampling strategy for formaldehyde

⎯ Part 3: Determination of formaldehyde and other carbonyl compounds — Active sampling method

⎯ Part 4: Determination of formaldehyde — Diffusive sampling method
⎯ Part 5: Sampling strategy for volatile organic compounds (VOCs)

⎯ 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/FID

⎯ Part 7: Sampling strategy for determination of airborne asbestos fibre concentrations

⎯ Part 8: Determination of local mean ages of air in buildings for characterizing ventilation conditions

⎯ Part 9: Determination of the emission of volatile organic compounds from building products and

furnishing — Emission test chamber method

⎯ Part 10: Determination of the emission of volatile organic compounds from building products and

furnishing — Emission test cell method

⎯ Part 11: Determination of the emission of volatile organic compounds from building products and

furnishing — Sampling, storage of samples and preparation of test specimens

⎯ Part 12: Sampling strategy for polychlorinated biphenyls (PCBs), polychlorinated dibenzo-p-dioxins

(PCDDs), polychlorinated dibenzofurans (PCDFs) and polycyclic aromatic hydrocarbons (PAHs)

⎯ Part 13: Determination of total (gas and particle-phase) polychlorinated dioxin-like biphenyls (PCBs) and

polychlorinated dibenzo-p-dioxins/dibenzofurans (PCDDs/PCDFs) — Collection on sorbent-backed filters

iv © ISO 2008 – All rights reserved
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ISO 16000-13:2008(E)

⎯ Part 14: Determination of total (gas and particle-phase) polychlorinated dioxin-like biphenyls (PCBs) and

polychlorinated dibenzo-p-dioxins/dibenzofurans (PCDDs/PCDFs) — Extraction, clean-up and analysis by

high-resolution gas chromatography and mass spectrometry
⎯ Part 15: Sampling strategy for nitrogen dioxide (NO )
⎯ Part 16: Detection and enumeration of moulds — Sampling by filtration
⎯ Part 17: Detection and enumeration of moulds — Culture-based method

⎯ Part 23: Performance test for evaluating the reduction of formaldehyde concentrations by sorptive

building materials

⎯ Part 24: Performance test for evaluating the reduction of volatile organic compounds and carbonyl

compounds without formaldehyde concentrations by sorptive building materials
The following parts are under preparation:
⎯ Part 18: Detection and enumeration of moulds — Sampling by impaction
⎯ Part 19: Sampling strategy for moulds

⎯ Part 25: Determination of the emission of semi-volatile organic compounds for building products —

Micro-chamber method
⎯ Part 26: Measurement strategy for carbon dioxide (CO )
⎯ Part 28: Sensory evaluation of emissions from building materials and products
The following parts are planned:
⎯ Part 20: Detection and enumeration of moulds — Sampling from house dust
⎯ Part 21: Detection and enumeration of moulds — Sampling from materials
⎯ Part 22: Detection and enumeration of moulds — Molecular methods

⎯ Part 27: Standard method for the quantitative analysis of asbestos fibres in settled dust

Furthermore,
[2]

⎯ ISO 12219-1 (under preparation), Indoor air — Road vehicles — Part 1: Whole vehicle test chamber —

Specification and method for the determination of volatile organic compounds in car interiors,

[3]

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

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

sampling, and
[4]

⎯ ISO 16017-2 , Indoor, ambient and workplace air — Sampling and analysis of volatile organic

compounds by sorbent tube/thermal desorption/capillary gas chromatography — Part 2: Diffusive

sampling
focus on volatile organic compound (VOC) measurements.
© ISO 2008 – All rights reserved v
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ISO 16000-13:2008(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).

This part of ISO 16000 is applicable to the collection from indoor air of dioxin-like polychlorinated biphenyls

(PCBs), polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) and to the

preparation of sampling media required for sampling. The same sampling methods described here are also

applicable to polycyclic aromatic hydrocarbons (PAHs) made up of two or more fused aromatic rings.

Procedures for preparation and extraction of sampling media for PAHs and for the analytical determination of

PAHs are given in ISO 12884, and therefore are not included here.

The sampling strategy to analyse PCBs, PCDDs/PCDFs and PAHs in indoor air is described in ISO 16000-12.

Several PCBs and PCDDs/PCDFs are considered to be potential human carcinogens. There are 209 individual

PCBs (congeners), 75 PCDDs and 135 PCDFs. The most toxic PCBs are those that are coplanar and

structurally similar to PCDDs. The most toxic PCDD is 2,3,7,8-tetrachlorodibenzodibenzo-p-dioxin

(2,3,7,8-TCDD).

PCBs are emitted into the indoor air primarily from concrete sealers, certain paints, or electrical capacitors, all

of which have been banned in recent years. The principal sources of PCDDs/PCDFs in indoor air are

impurities in wood preservatives containing pentachlorophenol (PCP) and emissions from fires involving

chlorinated products. Tracked-in soil and emissions from nearby landfills and abandoned industrial sites may

also contribute PCBs and PCDDs/PCDFs to the indoor environment.

Total PCB concentrations (six marker PCBs: PCB-28, -52, -101, -138, -153, and -180 multiplied by 5) in urban

outdoor air typically range from 10 to several hundred picograms per cubic metre (pg/m ). PCDDs/PCDFs are

usually found in urban outdoor air at extremely low concentrations; e.g. femtograms per cubic metre (fg/m ) to

picograms per cubic metre (pg/m ). PCBs and PCDDs/PCDFs may be distributed between the gas and

particle-associated phases in ambient or indoor air, depending on the temperature, humidity, degree of

chlorination, their concentration, and their capacity to associate with suspended particulate matter. These

compounds, especially those having vapour pressures above 10 kPa, will tend to vaporize from particle

filters during sampling. Consequently, a back-up sorbent trap is included for efficient sampling. Separate

analyses of the filter and sorbent trap will not reflect the original atmospheric phase distributions at normal

ambient temperatures because of volatilization of compounds from the filter and should not be attempted.

Shipping of PCDD/PCDF standards has to comply with the national legal regulations. They have to be

transported in special containers, which are commercially available. Handling should only be done by trained

operators.

This part of ISO 16000 describes sampling of polychlorinated dioxin-like biphenyls (PCBs) and polychlorinated

dibenzo-p-dioxins/dibenzofurans (PCDDs/PCDFs). Extraction, clean-up and analysis are described in

ISO 16000-14.
vi © ISO 2008 – All rights reserved
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INTERNATIONAL STANDARD ISO 16000-13:2008(E)
Indoor air —
Part 13:
Determination of total (gas and particle-phase) polychlorinated
dioxin-like biphenyls (PCBs) and polychlorinated
dibenzo-p-dioxins/dibenzofurans (PCDDs/PCDFs) — Collection
on sorbent-backed filters
1 Scope

This part of ISO 16000 specifies sampling and preparation of sampling media for dioxin-like polychlorinated

biphenyls (PCBs), polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) in

indoor air (see Table C.1). The method incorporates a sampling procedure that collects PCBs and

PCDFs/PCDDs from air on a fine-particle filter backed up by a sorbent trap. The method cannot be used to

separately determine gaseous PCBs and PCDFs/PCDDs and those that are particle-associated because

some of the compounds will volatilize from the filter and be collected by the sorbent trap. This part of

ISO 16000 does not address analytical methods for PCBs PCDDs and PCDFs, which are included in

ISO 16000-14. (ISO 16000-13 and ISO 16000-14 are both parts of the overall measurement procedure for the

determination of PCBs and PCDDs/PCDFs.)

Combined with the analytical procedures specified in ISO 16000-14, which incorporate specific analyses by

high-resolution gas chromatography combined with high-resolution mass spectrometry (HRGC/HRMS), this

method is capable of detecting 0,2 pg/m or lower concentrations of most PCBs and PCDFs/PCDDs. However,

it may not be possible to detect all analytes at 0,2 pg/m or lower, especially at lower sampling rates. To

achieve adequate detection limits, no less than 50 m of air should be sampled. For normal measurement

3 3

tasks, sampling volumes up to 360 m are employed (equivalent to a sampling period of 24 h at 16 m /h or 7 d

at 2 m /h). The method has been validated for sampling periods up to seven days. With the use of larger

sorbent traps, sampling volumes up to 1 000 m have been validated.

Sampling precision under normal conditions can be expected to be ± 25 % or better and uncertainty ± 50 % or

better.

If the appropriate restrictions are applied, this method can be used for small rooms, for example children’s

rooms as well as for offices.
2 Normative references

The following referenced documents are indispensable for the application 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 12884, Ambient air — Determination of total (gas and particle-phase) polycyclic aromatic

hydrocarbons — Collection on sorbent-backed filters with gas chromatographic/mass spectrometric analyses

ISO 16000-12, Indoor air — Part 12: Sampling strategy for polychlorinated biphenyls (PCBs), polychlorinated

dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs) and polycyclic aromatic hydrocarbons

(PAHs)
© ISO 2008 – All rights reserved 1
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ISO 16000-13:2008(E)

ISO 16000-14, Indoor air — Part 14: Determination of total (gas and particle-phase) polychlorinated dioxin-like

biphenyls (PCBs) and polychlorinated dibenzo-p-dioxins/dibenzofurans (PCDDs/PCDFs) — Extraction, clean-

up and analysis by high-resolution gas chromatography and mass spectrometry
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
sampling efficiency
% E
ability of the sampler to trap and retain targeted compounds

NOTE The % E is the percentage of the analyte of interest collected and retained by the sampling medium when it is

introduced into the air sampler and the sampler is operated under normal conditions for a period of time equal to or greater

than that required for the intended use.
3.2
dynamic retention efficiency

ability of the sampling medium to retain a given PCB, PCDD or PCDF that has been added to the sorbent trap

in a spiking solution when air is drawn through the sampler under normal conditions for a period of time equal

to or greater than that required for the intended use
3.3
dioxin-like PCB

non- and mono-ortho PCB having an affinity to the aryl hydrocarbon (Ah) receptor, showing similar

toxicological effects as the 2,3,7,8-substituted PCDDs/PCDFs according to WHO
NOTE 1 See Reference [5].
NOTE 2 See also Tables C.1 and C.2.
3.4
marker PCB
one of six PCBs

NOTE The six marker PCBs are PCB-28, PCB-52, PCB-101, PCB-138, PCB-153, and PCB-180.

3.5
spiking
addition of C -labelled PCB standards
3.6
operational performance characteristic

measurement that deals with the influence of the physical and chemical environment and maintenance

problems

EXAMPLE Main line voltage, temperature, supply of certain substances, set-up time, period of unattended operation

(see Reference [1]).
3.7
field blank

unexposed but spiked sample of the sampling medium [e.g. filter, polyurethane foam (PUF) trap, or complete

sampling cartridge], that is carried to the field and through the complete analytical procedure, including the

extraction, clean-up, and identification steps

NOTE The measurement value is needed to ensure that no significant contamination has occurred during all steps of

the measurement process and to check that the operator can achieve a quantification level adapted to the task.

2 © ISO 2008 – All rights reserved
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ISO 16000-13:2008(E)
3.8
analytical blank

unexposed but spiked sample of a reagent or sampling medium that is carried through the complete analytical

procedure including the extraction, clean-up and identification steps
3.9
sampling standard

marker agent that is added to a sampling medium before sampling to determine the overall efficiency of the

method
EXAMPLE C -labelled PCB and PCDD/PCDF.
3.10
extraction standard

marker agent, added to a sampling medium before extraction and used for calculation of results

EXAMPLE C -labelled PCB and PCDD/PCDF.
3.11
congener
substance which belongs to the chemical group of PCB or PCDD or PCDF

NOTE Includes the 209 individual PCBs, 75 individual PCDDs, and 135 individual PCDFs.

3.12
isomer
PCB or PCDD or PCDF with identical elemental composition but different structure
EXAMPLE 1-chlorobiphenyl and 2-chlorobiphenyl are isomers.
4 Abbreviated terms
(See also Tables C.1 and C.2.)
PCB polychlorinated biphenyl
PCDD polychlorinated dibenzo-p-dioxin
PCDF polychlorinated dibenzofuran
TeCB tetrachlorobiphenyl
PeCB pentachlorobiphenyl
HxCB hexachlorobiphenyl
HpCB heptachlorobiphenyl
TCDD tetrachlorodibenzo-p-dioxin
PeCDD pentachlorodibenzo-p-dioxin
HxCDD hexachlorodibenzo-p-dioxin
HpCDD heptachlorodibenzo-p-dioxin
OCDD octachlorodibenzo-p-dioxin
© ISO 2008 – All rights reserved 3
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ISO 16000-13:2008(E)
TCDF tetrachlorodibenzofuran
PeCDF pentachlorodibenzofuran
HxCDF hexachlorodibenzofuran
HpCDF heptachlorodibenzofuran
OCDF octachlorodibenzofuran
PTFE polytetrafluoroethylene
5 Principle

PCBs, PCDDs, and PCDFs are collected directly from indoor atmospheres by pulling a sample of air through

a fine particle filter backed up with a sorbent trap consisting of polyurethane foam (PUF). Low-volatility

compounds associated with airborne particulate matter are collected primarily on the particle filter. Gaseous

compounds that pass through the filter and compounds that vaporize from the filter are collected by the

polyurethane foam trap.

The method is applicable to rooms in residences, office buildings, and public or commercial facilities including

those with large interior spaces (e.g. factories, warehouses, enclosed stadiums). The sampling flow rate and

volume of air collected will depend on the size of the room or interior space being sampled. It may range from

3 3
1,5 m /h to 16 m /h according to the measurement task.

The sampling media (filter plus PUF) are combined and extracted together. Extraction procedures are

normally based on Soxhlet extraction with toluene or an equivalent solvent. C -labelled PCB/PCDD/PCDF

standards are added before sampling and extraction to monitor sampling efficiency and recovery. Spiking with

C -labelled PCBs/PCDDs/PCDFs before sampling is necessary to determine the overall recoveries of the

PCB/PCDD/PCDF congeners. Losses during extraction and clean-up are detected and compensated by using

these isotopically-labelled surrogates as internal extraction standards for quantification, together with recovery

standards that are added just before the HRGC/HRMS analysis.
6 Apparatus and materials
6.1 Sampling apparatus

A schematic of a typical sampling system is shown in Figure 1 and that of a typical sampling module is shown

in Figure 2.

The sampling module shown in Figure 2 is the basis of the outdoor sampler for polycyclic aromatic

hydrocarbons (PAHs) described in ISO 12884. It is based on a published design (Reference [6]) and is also

used for determination of PCDDs and PCDFs in ambient air (Reference [7]). A module of this design having

the same dimensions as those described in ISO 12884 may be used for sampling rates from 1,5 m /h to

3 3

16 m /h and total air volumes up to 360 m depending on the capacity of the air sampling system used.

Modules of this basic design having various dimensions and configurations may be used if validated.

NOTE The particle capture velocity of a sampler will depend on the face velocity during sampling. For example, it can

be estimated by Stokes Law that pulling air through a 100 mm filter at 15 m /h will collect particles smaller than about

40 µm. At a sampling rate of 6 m /h, particles less than about 20 µm would be captured. Reducing the sampling rate

further to 1,5 m /h would collect particles smaller than 10 µm to 12 µm. Experience shows for indoor air measurements

that there is little or no significant differences in what is measured with the same sampling module at different flow rates

down to 1,5 m /h. Likewise, if a size-selective inlet (e.g. PM or PM ) is used, there should be little effect on the total

2,5 10

PCB/PCDD/PCDF content of the sample unless there is a nearby emission source of particle-associated compounds.

4 © ISO 2008 – All rights reserved
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ISO 16000-13:2008(E)
3 3

There are a number of sampling systems capable of providing air flows from 1,5 m /h to 16 m /h, some of

which may have air flow controls that can be set over a wide range to provide the desired sampling rate.

Limitations on permissible air sampling rates and volumes are discussed in Clause 8. Some examples of

sampling systems are presented in Annex A.
Key
1 sampling module (see Figure 2)
2 air sampling pump
3 timer
4 flow controller (with measuring electronics)
5 elapsed time counter
Air intake.
Exhaust.
Figure 1 — Schematic drawing of a typical sampling system
© ISO 2008 – All rights reserved 5
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ISO 16000-13:2008(E)
a) Typical sampling module b) Exploded assembly drawing
Key
1 air flow inlet 8 filter support screen
2 filter support screen (identical to 8) 9 filter holder
3 assembled sampling module 10 glass sorbent cartridge (PUF trap)
4 air flow exhaust 11 PUF trap
5 filter retainer 12 support screen cartridge holder
6 sealing gaskets 13 cartridge holder
7 quartz- or glass-fibre filter
Figure 2 — Typical sampling module that integrates particle filter and PUF trap
6 © ISO 2008 – All rights reserved
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ISO 16000-13:2008(E)
6.2 Sampling materials

6.2.1 Polyurethane foam, open-cell, polyether type, density 22 mg/cm , cut into cylinders 76 mm

long × 62 mm diameter, or other appropriate size depending on the specific sampling module used. They are

available from several commercial sources. The PUF cylinders should be slightly larger in diameter than the

internal diameter of the sorbent cartridge so that the sampled air does not flow around it instead of through it.

Cleaning is performed according to Clause 7.

6.2.2 Filter, micro-quartz- or glass-fibre, binderless, acid-washed, with a filtration efficiency of 99,99 %

mass fraction or better for particles below 0,5 µm, or other appropriate size filter depending on the specific

sampling module used. This efficiency shall be certified by the filter supplier.
6.2.3 C-labelled sampling standards, see Tables 1 and 2 for composition.

6.2.4 Aluminium foil, for packing the filters and PUF traps before and after sampling.

6.2.5 Forceps and latex or neoprene gloves, for handling the filter and PUF traps.

6.2.6 Microlitre syringes, for applying recovery standards on the filter media.

6.2.7 PTFE tape, for sealing the suction tube in the screw-in port of the protective housing.

6.2.8 Glass jar or other suitable containers, sealable, for storing and transporting PUF traps and particle

filters.
6.2.9 Desiccator or vacuum drying cabinet.
6.2.10 Diaphragm pump or other suitable pump.
6.3 Analytical reagents
6.3.1 Toluene, glass distilled, chromatographic or pesticide quality.
6.3.2 n-hexane, glass distilled, chromatographic or pesticide quality.
6.3.3 Dichloromethane, glass distilled, chromatographic or pesticide quality.
6.3.4 Acetone, glass distilled, chromatographic or pesticide quality.
6.3.5 n-nonane, glass distilled, chromatographic or pesticide quality.

6.3.6 n-tetradecane (keeper), glass distilled, chromatographic or pesticide quality.

6.3.7 C -labelled extraction standards, see Tables 1 and 2 for composition (see 6.4).

6.3.8 C -labelled injection standards, see Tables 1 and 2 for composition (see 6.4).

© ISO 2008 – All rights reserved 7
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ISO 16000-13:2008(E)
6.4 C -labelled standards

The masses of C -labelled sampling standards in 100 µl of appropriate solvent (e.g. toluene or 4 %

n-tetradecane/n-nonane) that should be added to each sample at a concentration level of approximately

3 3

100 fg of TEQ/m for an approximately 180 m of sampling volume are listed in Table 1 (PCDDs/PCDFs) and

Table 2 (PCBs). For TEQ and WHO-TEQ , see Clause C.3.
PCB

The extraction standards should be added to the various sampling media immediately after the samples are

received in the laboratory. The C -labelled congeners are used for quantification because they behave

exactly like the extracted native PCBs/PCDDs/PCDFs during the clean-up, due to their nearly identical

chemical and physical properties. The injection standards (see Table 1) are for determining the recovery rates.

The masses specified in Table 1 and Table 2 of standards to be used shall to be adjusted appropriately if

considerably higher masses of native PCBs/PCDDs/PCDFs are expected in the sample. The use and

handling of the extraction and recovery standards are described in ISO 16000-14.

Table 1 — C -labelled 2,3,7,8-PCDD/PCDF congeners for addition to samples before sampling,

3 3

extraction and GC injection to measure approximately 100 fg TEQ/m and approximately 180 m

sampling volume
Solution to be added before:
Solution: Sampling Extraction GC-Injection
(sampling standard) (extraction standard) (recovery standard)
Total volume in µl:
(e.g. in toluene, n-nonane) 100 100 25
Congeners added Total mass
13 a
C-2,3,7,8-TCDF 25
C-1,2,3,4-TCDD 25
13 a
C-2,3,7,8-TCDD 25
C-1,2,3,7,8-PeCDF 25
13 a
C-2,3,4,7,8-PeCDF 25
13 a
C-1,2,3,7,8-PeCDD 25
13 a
C-1,2,3,4,7,8-HxCDF 25
C-1,2,3,6,7,8-HxCDF 25
C-1,2,3,7,8,9-HxCDF 25
C-,2,3,4,6,7,8-HxCDF 25
C -1,2,3,4,7,8-HxCDD 25
13 a
C -1,2,3,6,7,8-HxCDD 25
C -1,2,3,7,8,9-HxCDD 25
13 a
C -1,2,3,4,6,7,8-HpCDF 50
C -1,2,3,4,7,8,9-HpCDF50
13 a
C -1,2,3,4,6,7,8-HpCDD 50
C -OCDF 50
C -OCDD 50

These standards are used to quantify the remaining congeners of the associated groups of chlorinated homologues for which no

standard was added.
8 © ISO 2008 – All rights reserved
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ISO 16000-13:2008(E)

Table 2 — C -labelled PCBs congeners to be added to the sample at different stages of th

...

SLOVENSKI STANDARD
SIST ISO 16000-13:2013
01-december-2013

1RWUDQML]UDNGHO'RORþHYDQMHFHORWQLK YSOLQLKLQGHOFLK SROLNORULUDQLK

GLRNVLQXSRGREQLKELIHQLORY 3&% LQSROLNORULUDQLKGLEHQ]RS
GLRNVLQRYGLEHQ]RIXUDQRY 3&''3&') =ELUDQMHQDILOWULK]DEVRUEHQWRP

Indoor air - Part 13: Determination of total (gas and particle-phase) polychlorinated dioxin

-like biphenyls (PCBs) and polychlorinated dibenzo-p-dioxins/dibenzofurans
(PCDDs/PCDFs) - Collection on sorbent-backed filters

Air intérieur - Partie 13: Dosage des polychlorobiphényles (PCB) de type dioxine et des

polychlorodibenzo-p-dioxines (PCDD)/polychlorodibenzofuranes (PCDF) totaux (en
phase gazeuse et en phase particulaire) - Collecte sur des filtres adsorbants
Ta slovenski standard je istoveten z: ISO 16000-13:2008
ICS:
13.040.20 Kakovost okoljskega zraka Ambient atmospheres
SIST ISO 16000-13:2013 en,fr

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

---------------------- Page: 1 ----------------------
SIST ISO 16000-13:2013
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SIST ISO 16000-13:2013
INTERNATIONAL ISO
STANDARD 16000-13
First edition
2008-11-01
Indoor air —
Part 13:
Determination of total (gas and particle-
phase) polychlorinated dioxin-like
biphenyls (PCBs) and polychlorinated
dibenzo-p-dioxins/dibenzofurans
(PCDDs/PCDFs) — Collection on sorbent-
backed filters
Air intérieur —
Partie 13: Dosage des polychlorobiphényles (PCB) de type dioxine et
des polychlorodibenzo-p-dioxines (PCDD)/polychlorodibenzofuranes
(PCDF) totaux (en phase gazeuse et en phase particulaire) — Collecte
sur des filtres adsorbants
Reference number
ISO 16000-13:2008(E)
ISO 2008
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SIST ISO 16000-13:2013
ISO 16000-13:2008(E)
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Published in Switzerland
ii © ISO 2008 – All rights reserved
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SIST ISO 16000-13:2013
ISO 16000-13:2008(E)
Contents Page

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

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

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

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

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

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

5 Principle..................................................................................................................................................4

6 Apparatus and materials.......................................................................................................................4

7 Preparation of sampling media............................................................................................................9

8 Sampling...............................................................................................................................................10

9 Minimum requirements for sampling ................................................................................................12

Annex A (informative) Details of samplers.....................................................................................................13

Annex B (normative) Determination of sampling efficiency or dynamic retention efficiency..................24

Annex C (informative) Structure, toxicity and calculation of toxicity equivalents.....................................25

Bibliography......................................................................................................................................................30

© ISO 2008 – All rights reserved iii
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SIST ISO 16000-13:2013
ISO 16000-13:2008(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 2.

The main task of technical committees is to prepare International Standards. 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 document may be the subject of patent

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

ISO 16000-13 was prepared by Technical Committee ISO/TC 146, Air quality, Subcommittee SC 6, Indoor air.

ISO 16000 consists of the following parts, under the general title Indoor air:
⎯ Part 1: General aspects of sampling strategy
⎯ Part 2: Sampling strategy for formaldehyde

⎯ Part 3: Determination of formaldehyde and other carbonyl compounds — Active sampling method

⎯ Part 4: Determination of formaldehyde — Diffusive sampling method
⎯ Part 5: Sampling strategy for volatile organic compounds (VOCs)

⎯ 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/FID

⎯ Part 7: Sampling strategy for determination of airborne asbestos fibre concentrations

⎯ Part 8: Determination of local mean ages of air in buildings for characterizing ventilation conditions

⎯ Part 9: Determination of the emission of volatile organic compounds from building products and

furnishing — Emission test chamber method

⎯ Part 10: Determination of the emission of volatile organic compounds from building products and

furnishing — Emission test cell method

⎯ Part 11: Determination of the emission of volatile organic compounds from building products and

furnishing — Sampling, storage of samples and preparation of test specimens

⎯ Part 12: Sampling strategy for polychlorinated biphenyls (PCBs), polychlorinated dibenzo-p-dioxins

(PCDDs), polychlorinated dibenzofurans (PCDFs) and polycyclic aromatic hydrocarbons (PAHs)

⎯ Part 13: Determination of total (gas and particle-phase) polychlorinated dioxin-like biphenyls (PCBs) and

polychlorinated dibenzo-p-dioxins/dibenzofurans (PCDDs/PCDFs) — Collection on sorbent-backed filters

iv © ISO 2008 – All rights reserved
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SIST ISO 16000-13:2013
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⎯ Part 14: Determination of total (gas and particle-phase) polychlorinated dioxin-like biphenyls (PCBs) and

polychlorinated dibenzo-p-dioxins/dibenzofurans (PCDDs/PCDFs) — Extraction, clean-up and analysis by

high-resolution gas chromatography and mass spectrometry
⎯ Part 15: Sampling strategy for nitrogen dioxide (NO )
⎯ Part 16: Detection and enumeration of moulds — Sampling by filtration
⎯ Part 17: Detection and enumeration of moulds — Culture-based method

⎯ Part 23: Performance test for evaluating the reduction of formaldehyde concentrations by sorptive

building materials

⎯ Part 24: Performance test for evaluating the reduction of volatile organic compounds and carbonyl

compounds without formaldehyde concentrations by sorptive building materials
The following parts are under preparation:
⎯ Part 18: Detection and enumeration of moulds — Sampling by impaction
⎯ Part 19: Sampling strategy for moulds

⎯ Part 25: Determination of the emission of semi-volatile organic compounds for building products —

Micro-chamber method
⎯ Part 26: Measurement strategy for carbon dioxide (CO )
⎯ Part 28: Sensory evaluation of emissions from building materials and products
The following parts are planned:
⎯ Part 20: Detection and enumeration of moulds — Sampling from house dust
⎯ Part 21: Detection and enumeration of moulds — Sampling from materials
⎯ Part 22: Detection and enumeration of moulds — Molecular methods

⎯ Part 27: Standard method for the quantitative analysis of asbestos fibres in settled dust

Furthermore,
[2]

⎯ ISO 12219-1 (under preparation), Indoor air — Road vehicles — Part 1: Whole vehicle test chamber —

Specification and method for the determination of volatile organic compounds in car interiors,

[3]

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

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

sampling, and
[4]

⎯ ISO 16017-2 , Indoor, ambient and workplace air — Sampling and analysis of volatile organic

compounds by sorbent tube/thermal desorption/capillary gas chromatography — Part 2: Diffusive

sampling
focus on volatile organic compound (VOC) measurements.
© ISO 2008 – All rights reserved v
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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).

This part of ISO 16000 is applicable to the collection from indoor air of dioxin-like polychlorinated biphenyls

(PCBs), polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) and to the

preparation of sampling media required for sampling. The same sampling methods described here are also

applicable to polycyclic aromatic hydrocarbons (PAHs) made up of two or more fused aromatic rings.

Procedures for preparation and extraction of sampling media for PAHs and for the analytical determination of

PAHs are given in ISO 12884, and therefore are not included here.

The sampling strategy to analyse PCBs, PCDDs/PCDFs and PAHs in indoor air is described in ISO 16000-12.

Several PCBs and PCDDs/PCDFs are considered to be potential human carcinogens. There are 209 individual

PCBs (congeners), 75 PCDDs and 135 PCDFs. The most toxic PCBs are those that are coplanar and

structurally similar to PCDDs. The most toxic PCDD is 2,3,7,8-tetrachlorodibenzodibenzo-p-dioxin

(2,3,7,8-TCDD).

PCBs are emitted into the indoor air primarily from concrete sealers, certain paints, or electrical capacitors, all

of which have been banned in recent years. The principal sources of PCDDs/PCDFs in indoor air are

impurities in wood preservatives containing pentachlorophenol (PCP) and emissions from fires involving

chlorinated products. Tracked-in soil and emissions from nearby landfills and abandoned industrial sites may

also contribute PCBs and PCDDs/PCDFs to the indoor environment.

Total PCB concentrations (six marker PCBs: PCB-28, -52, -101, -138, -153, and -180 multiplied by 5) in urban

outdoor air typically range from 10 to several hundred picograms per cubic metre (pg/m ). PCDDs/PCDFs are

usually found in urban outdoor air at extremely low concentrations; e.g. femtograms per cubic metre (fg/m ) to

picograms per cubic metre (pg/m ). PCBs and PCDDs/PCDFs may be distributed between the gas and

particle-associated phases in ambient or indoor air, depending on the temperature, humidity, degree of

chlorination, their concentration, and their capacity to associate with suspended particulate matter. These

compounds, especially those having vapour pressures above 10 kPa, will tend to vaporize from particle

filters during sampling. Consequently, a back-up sorbent trap is included for efficient sampling. Separate

analyses of the filter and sorbent trap will not reflect the original atmospheric phase distributions at normal

ambient temperatures because of volatilization of compounds from the filter and should not be attempted.

Shipping of PCDD/PCDF standards has to comply with the national legal regulations. They have to be

transported in special containers, which are commercially available. Handling should only be done by trained

operators.

This part of ISO 16000 describes sampling of polychlorinated dioxin-like biphenyls (PCBs) and polychlorinated

dibenzo-p-dioxins/dibenzofurans (PCDDs/PCDFs). Extraction, clean-up and analysis are described in

ISO 16000-14.
vi © ISO 2008 – All rights reserved
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SIST ISO 16000-13:2013
INTERNATIONAL STANDARD ISO 16000-13:2008(E)
Indoor air —
Part 13:
Determination of total (gas and particle-phase) polychlorinated
dioxin-like biphenyls (PCBs) and polychlorinated
dibenzo-p-dioxins/dibenzofurans (PCDDs/PCDFs) — Collection
on sorbent-backed filters
1 Scope

This part of ISO 16000 specifies sampling and preparation of sampling media for dioxin-like polychlorinated

biphenyls (PCBs), polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) in

indoor air (see Table C.1). The method incorporates a sampling procedure that collects PCBs and

PCDFs/PCDDs from air on a fine-particle filter backed up by a sorbent trap. The method cannot be used to

separately determine gaseous PCBs and PCDFs/PCDDs and those that are particle-associated because

some of the compounds will volatilize from the filter and be collected by the sorbent trap. This part of

ISO 16000 does not address analytical methods for PCBs PCDDs and PCDFs, which are included in

ISO 16000-14. (ISO 16000-13 and ISO 16000-14 are both parts of the overall measurement procedure for the

determination of PCBs and PCDDs/PCDFs.)

Combined with the analytical procedures specified in ISO 16000-14, which incorporate specific analyses by

high-resolution gas chromatography combined with high-resolution mass spectrometry (HRGC/HRMS), this

method is capable of detecting 0,2 pg/m or lower concentrations of most PCBs and PCDFs/PCDDs. However,

it may not be possible to detect all analytes at 0,2 pg/m or lower, especially at lower sampling rates. To

achieve adequate detection limits, no less than 50 m of air should be sampled. For normal measurement

3 3

tasks, sampling volumes up to 360 m are employed (equivalent to a sampling period of 24 h at 16 m /h or 7 d

at 2 m /h). The method has been validated for sampling periods up to seven days. With the use of larger

sorbent traps, sampling volumes up to 1 000 m have been validated.

Sampling precision under normal conditions can be expected to be ± 25 % or better and uncertainty ± 50 % or

better.

If the appropriate restrictions are applied, this method can be used for small rooms, for example children’s

rooms as well as for offices.
2 Normative references

The following referenced documents are indispensable for the application 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 12884, Ambient air — Determination of total (gas and particle-phase) polycyclic aromatic

hydrocarbons — Collection on sorbent-backed filters with gas chromatographic/mass spectrometric analyses

ISO 16000-12, Indoor air — Part 12: Sampling strategy for polychlorinated biphenyls (PCBs), polychlorinated

dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs) and polycyclic aromatic hydrocarbons

(PAHs)
© ISO 2008 – All rights reserved 1
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ISO 16000-14, Indoor air — Part 14: Determination of total (gas and particle-phase) polychlorinated dioxin-like

biphenyls (PCBs) and polychlorinated dibenzo-p-dioxins/dibenzofurans (PCDDs/PCDFs) — Extraction, clean-

up and analysis by high-resolution gas chromatography and mass spectrometry
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
sampling efficiency
% E
ability of the sampler to trap and retain targeted compounds

NOTE The % E is the percentage of the analyte of interest collected and retained by the sampling medium when it is

introduced into the air sampler and the sampler is operated under normal conditions for a period of time equal to or greater

than that required for the intended use.
3.2
dynamic retention efficiency

ability of the sampling medium to retain a given PCB, PCDD or PCDF that has been added to the sorbent trap

in a spiking solution when air is drawn through the sampler under normal conditions for a period of time equal

to or greater than that required for the intended use
3.3
dioxin-like PCB

non- and mono-ortho PCB having an affinity to the aryl hydrocarbon (Ah) receptor, showing similar

toxicological effects as the 2,3,7,8-substituted PCDDs/PCDFs according to WHO
NOTE 1 See Reference [5].
NOTE 2 See also Tables C.1 and C.2.
3.4
marker PCB
one of six PCBs

NOTE The six marker PCBs are PCB-28, PCB-52, PCB-101, PCB-138, PCB-153, and PCB-180.

3.5
spiking
addition of C -labelled PCB standards
3.6
operational performance characteristic

measurement that deals with the influence of the physical and chemical environment and maintenance

problems

EXAMPLE Main line voltage, temperature, supply of certain substances, set-up time, period of unattended operation

(see Reference [1]).
3.7
field blank

unexposed but spiked sample of the sampling medium [e.g. filter, polyurethane foam (PUF) trap, or complete

sampling cartridge], that is carried to the field and through the complete analytical procedure, including the

extraction, clean-up, and identification steps

NOTE The measurement value is needed to ensure that no significant contamination has occurred during all steps of

the measurement process and to check that the operator can achieve a quantification level adapted to the task.

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3.8
analytical blank

unexposed but spiked sample of a reagent or sampling medium that is carried through the complete analytical

procedure including the extraction, clean-up and identification steps
3.9
sampling standard

marker agent that is added to a sampling medium before sampling to determine the overall efficiency of the

method
EXAMPLE C -labelled PCB and PCDD/PCDF.
3.10
extraction standard

marker agent, added to a sampling medium before extraction and used for calculation of results

EXAMPLE C -labelled PCB and PCDD/PCDF.
3.11
congener
substance which belongs to the chemical group of PCB or PCDD or PCDF

NOTE Includes the 209 individual PCBs, 75 individual PCDDs, and 135 individual PCDFs.

3.12
isomer
PCB or PCDD or PCDF with identical elemental composition but different structure
EXAMPLE 1-chlorobiphenyl and 2-chlorobiphenyl are isomers.
4 Abbreviated terms
(See also Tables C.1 and C.2.)
PCB polychlorinated biphenyl
PCDD polychlorinated dibenzo-p-dioxin
PCDF polychlorinated dibenzofuran
TeCB tetrachlorobiphenyl
PeCB pentachlorobiphenyl
HxCB hexachlorobiphenyl
HpCB heptachlorobiphenyl
TCDD tetrachlorodibenzo-p-dioxin
PeCDD pentachlorodibenzo-p-dioxin
HxCDD hexachlorodibenzo-p-dioxin
HpCDD heptachlorodibenzo-p-dioxin
OCDD octachlorodibenzo-p-dioxin
© ISO 2008 – All rights reserved 3
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SIST ISO 16000-13:2013
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TCDF tetrachlorodibenzofuran
PeCDF pentachlorodibenzofuran
HxCDF hexachlorodibenzofuran
HpCDF heptachlorodibenzofuran
OCDF octachlorodibenzofuran
PTFE polytetrafluoroethylene
5 Principle

PCBs, PCDDs, and PCDFs are collected directly from indoor atmospheres by pulling a sample of air through

a fine particle filter backed up with a sorbent trap consisting of polyurethane foam (PUF). Low-volatility

compounds associated with airborne particulate matter are collected primarily on the particle filter. Gaseous

compounds that pass through the filter and compounds that vaporize from the filter are collected by the

polyurethane foam trap.

The method is applicable to rooms in residences, office buildings, and public or commercial facilities including

those with large interior spaces (e.g. factories, warehouses, enclosed stadiums). The sampling flow rate and

volume of air collected will depend on the size of the room or interior space being sampled. It may range from

3 3
1,5 m /h to 16 m /h according to the measurement task.

The sampling media (filter plus PUF) are combined and extracted together. Extraction procedures are

normally based on Soxhlet extraction with toluene or an equivalent solvent. C -labelled PCB/PCDD/PCDF

standards are added before sampling and extraction to monitor sampling efficiency and recovery. Spiking with

C -labelled PCBs/PCDDs/PCDFs before sampling is necessary to determine the overall recoveries of the

PCB/PCDD/PCDF congeners. Losses during extraction and clean-up are detected and compensated by using

these isotopically-labelled surrogates as internal extraction standards for quantification, together with recovery

standards that are added just before the HRGC/HRMS analysis.
6 Apparatus and materials
6.1 Sampling apparatus

A schematic of a typical sampling system is shown in Figure 1 and that of a typical sampling module is shown

in Figure 2.

The sampling module shown in Figure 2 is the basis of the outdoor sampler for polycyclic aromatic

hydrocarbons (PAHs) described in ISO 12884. It is based on a published design (Reference [6]) and is also

used for determination of PCDDs and PCDFs in ambient air (Reference [7]). A module of this design having

the same dimensions as those described in ISO 12884 may be used for sampling rates from 1,5 m /h to

3 3

16 m /h and total air volumes up to 360 m depending on the capacity of the air sampling system used.

Modules of this basic design having various dimensions and configurations may be used if validated.

NOTE The particle capture velocity of a sampler will depend on the face velocity during sampling. For example, it can

be estimated by Stokes Law that pulling air through a 100 mm filter at 15 m /h will collect particles smaller than about

40 µm. At a sampling rate of 6 m /h, particles less than about 20 µm would be captured. Reducing the sampling rate

further to 1,5 m /h would collect particles smaller than 10 µm to 12 µm. Experience shows for indoor air measurements

that there is little or no significant differences in what is measured with the same sampling module at different flow rates

down to 1,5 m /h. Likewise, if a size-selective inlet (e.g. PM or PM ) is used, there should be little effect on the total

2,5 10

PCB/PCDD/PCDF content of the sample unless there is a nearby emission source of particle-associated compounds.

4 © ISO 2008 – All rights reserved
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3 3

There are a number of sampling systems capable of providing air flows from 1,5 m /h to 16 m /h, some of

which may have air flow controls that can be set over a wide range to provide the desired sampling rate.

Limitations on permissible air sampling rates and volumes are discussed in Clause 8. Some examples of

sampling systems are presented in Annex A.
Key
1 sampling module (see Figure 2)
2 air sampling pump
3 timer
4 flow controller (with measuring electronics)
5 elapsed time counter
Air intake.
Exhaust.
Figure 1 — Schematic drawing of a typical sampling system
© ISO 2008 – All rights reserved 5
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SIST ISO 16000-13:2013
ISO 16000-13:2008(E)
a) Typical sampling module b) Exploded assembly drawing
Key
1 air flow inlet 8 filter support screen
2 filter support screen (identical to 8) 9 filter holder
3 assembled sampling module 10 glass sorbent cartridge (PUF trap)
4 air flow exhaust 11 PUF trap
5 filter retainer 12 support screen cartridge holder
6 sealing gaskets 13 cartridge holder
7 quartz- or glass-fibre filter
Figure 2 — Typical sampling module that integrates particle filter and PUF trap
6 © ISO 2008 – All rights reserved
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SIST ISO 16000-13:2013
ISO 16000-13:2008(E)
6.2 Sampling materials

6.2.1 Polyurethane foam, open-cell, polyether type, density 22 mg/cm , cut into cylinders 76 mm

long × 62 mm diameter, or other appropriate size depending on the specific sampling module used. They are

available from several commercial sources. The PUF cylinders should be slightly larger in diameter than the

internal diameter of the sorbent cartridge so that the sampled air does not flow around it instead of through it.

Cleaning is performed according to Clause 7.

6.2.2 Filter, micro-quartz- or glass-fibre, binderless, acid-washed, with a filtration efficiency of 99,99 %

mass fraction or better for particles below 0,5 µm, or other appropriate size filter depending on the specific

sampling module used. This efficiency shall be certified by the filter supplier.
6.2.3 C-labelled sampling standards, see Tables 1 and 2 for composition.

6.2.4 Aluminium foil, for packing the filters and PUF traps before and after sampling.

6.2.5 Forceps and latex or neoprene gloves, for handling the filter and PUF traps.

6.2.6 Microlitre syringes, for applying recovery standards on the filter media.

6.2.7 PTFE tape, for sealing the suction tube in the screw-in port of the protective housing.

6.2.8 Glass jar or other suitable containers, sealable, for storing and transporting PUF traps and particle

filters.
6.2.9 Desiccator or vacuum drying cabinet.
6.2.10 Diaphragm pump or other suitable pump.
6.3 Analytical reagents
6.3.1 Toluene, glass distilled, chromatographic or pesticide quality.
6.3.2 n-hexane, glass distilled, chromatographic or pesticide quality.
6.3.3 Dichloromethane, glass distilled, chromatographic or pesticide quality.
6.3.4 Acetone, glass distilled, chromatographic or pesticide quality.
6.3.5 n-nonane, glass distilled, chromatographic or pesticide quality.

6.3.6 n-tetradecane (keeper), glass distilled, chromatographic or pesticide quality.

6.3.7 C -labelled extraction standards, see Tables 1 and 2 for composition (see 6.4).

6.3.8 C -labelled injection standards, see Tables 1 and 2 for composition (see 6.4).

© ISO 2008 – All rights reserved 7
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SIST ISO 16000-13:2013
ISO 16000-13:2008(E)
6.4 C -labelled standards

The masses of C -labelled sampling standards in 100 µl of appropriate solvent (e.g. toluene or 4 %

n-tetradecane/n-nonane) that should be added to each sample at a concentration level of approximately

3 3

100 fg of TEQ/m for an approximately 180 m of sampling volume are listed in Table 1 (PCDDs/PCDFs) and

Table 2 (PCBs). For TEQ and WHO-TEQ , see Clause C.3.
PCB

The extraction standards should be added to the various sampling media immediately after the samples are

received in the laboratory. The C -labelled congeners are used for quantification because they behave

exactly like the extracted native PCBs/PCDDs/PCDFs during the clean-up, due to their nearly identical

chemical and physical properties. The injection standards (see Table 1) are for determining the recovery rates.

The masses specified in Table 1 and Table 2 of standards to be used shall to be adjusted appropriately if

considerably higher masses of native PCBs/PCDDs/P
...

NORME ISO
INTERNATIONALE 16000-13
Première édition
2008-11-01
Air intérieur —
Partie 13:
Dosage des polychlorobiphényles (PCB)
de type dioxine et des
polychlorodibenzo-p-dioxines
(PCDD)/polychlorodibenzofuranes (PCDF)
totaux (en phase gazeuse et en phase
particulaire) — Collecte sur des filtres
adsorbants
Indoor air —
Part 13: Determination of total (gas and particle-phase) polychlorinated
dioxin-like biphenyls (PCBs) and polychlorinated
dibenzo-p-dioxins/dibenzofurans (PCDDs/PCDFs) — Collection on
sorbent-backed filters
Numéro de référence
ISO 16000-13:2008(F)
ISO 2008
---------------------- Page: 1 ----------------------
ISO 16000-13:2008(F)
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Publié en Suisse
ii © ISO 2008 – Tous droits réservés
---------------------- Page: 2 ----------------------
ISO 16000-13:2008(F)
Sommaire Page

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

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

1 Domaine d'application ..........................................................................................................................1

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

3 Termes et définitions ............................................................................................................................2

4 Termes abrégés .....................................................................................................................................4

5 Principe...................................................................................................................................................4

6 Appareillage et matériels......................................................................................................................5

7 Préparation des supports d'échantillonnage ...................................................................................10

8 Échantillonnage...................................................................................................................................11

9 Exigences minimales pour l'échantillonnage...................................................................................13

Annexe A (informative) Description des échantillonneurs...........................................................................14

Annexe B (normative) Détermination de l'efficacité de prélèvement ou de l'efficacité de rétention

dynamique............................................................................................................................................26

Annexe C (informative) Structure, toxicité et calcul des équivalents toxiques..........................................28

Bibliographie.....................................................................................................................................................33

© ISO 2008 – Tous droits réservés iii
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ISO 16000-13:2008(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 (CEI) en ce qui concerne la normalisation électrotechnique.

Les Normes internationales sont rédigées conformément aux règles données dans les Directives ISO/CEI,

Partie 2.

La tâche principale des comités techniques est d'élaborer les Normes internationales. Les projets de Normes

internationales adoptés par les comités techniques sont soumis aux comités membres pour vote. Leur

publication comme Normes internationales requiert l'approbation de 75 % au moins des comités membres

votants.

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.

L'ISO 16000-13 a été élaborée par le comité technique ISO/TC 146, Qualité de l'air, sous-comité SC 6, Air

intérieur.

L'ISO 16000 comprend les parties suivantes, présentées sous le titre général Air intérieur:

⎯ Partie 1: Aspects généraux de la stratégie d'échantillonnage
⎯ Partie 2: Stratégie d'échantillonnage du formaldéhyde

⎯ Partie 3: Dosage du formaldéhyde et d'autres composés carbonylés — Méthode par échantillonnage actif

⎯ Partie 4: Dosage du formaldéhyde — Méthode par échantillonnage diffusif

⎯ Partie 5: Stratégie d'échantillonnage pour les composés organiques volatils (COV)

⎯ Partie 6: Dosage des composés organiques volatils dans l'air intérieur des locaux et enceintes d'essai par

échantillonnage actif sur le sorbant Tenax TA , désorption thermique et chromatographie en phase

gazeuse utilisant MS/FID

⎯ Partie 7: Stratégie d'échantillonnage pour la détermination des concentrations en fibres d'amiante en

suspension dans l'air

⎯ Partie 8: Détermination des âges moyens locaux de l'air dans des bâtiments pour caractériser les

conditions de ventilation

⎯ Partie 9: Dosage de l'émission de composés organiques volatils de produits de construction et d'objets

d'équipement — Méthode de la chambre d'essai d'émission

⎯ Partie 10: Dosage de l'émission de composés organiques volatils de produits de construction et d'objets

d'équipement — Méthode de la cellule d'essai d'émission

⎯ Partie 11: Dosage de l'émission de composés organiques volatils de produits de construction et d'objets

d'équipement — Échantillonnage, conservation des échantillons et préparation d'échantillons pour essai

⎯ Partie 12: Stratégie d'échantillonnage des polychlorobiphényles (PCB), des polychlorodibenzo-p-dioxines

(PCDD), des polychlorodibenzofuranes, (PCDF) et des hydrocarbures aromatiques polycycliques (HAP)

iv © ISO 2008 – Tous droits réservés
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ISO 16000-13:2008(F)

⎯ Partie 13: Dosage des polychlorobiphényles (PCB) de type dioxine et des polychlorodibenzo-p-dioxines

(PCDD)/polychlorodibenzofuranes (PCDF) totaux (en phase gazeuse et en phase particulaire) —

Collecte sur des filtres adsorbants

⎯ Partie 14: Dosage des polychlorobiphényles (PCB) de type dioxine et des polychlorodibenzo-p-dioxines

(PCDD)/polychlorodibenzofuranes (PCDF) totaux (en phase gazeuse et en phase particulaire) —

Extraction, purification et analyse par chromatographie en phase gazeuse haute résolution et

spectrométrie de masse
⎯ Partie 15: Stratégie d'échantillonnage du dioxyde d'azote (NO )

⎯ Partie 16: Détection et dénombrement des moisissures — Échantillonnage par filtration

⎯ Partie 17: Détection et dénombrement des moisissures — Méthode par culture

⎯ Partie 23: Essai de performance pour l'évaluation de la réduction des concentrations en formaldéhyde

par des matériaux de construction sorptifs

⎯ Partie 24: Essai de performance pour l'évaluation de la réduction des concentrations en composés

organiques volatils et en composés carbonyles sans formaldéhyde, par des matériaux de construction

sorptifs
Les parties suivantes sont en cours de préparation:

⎯ Partie 18: Détection et dénombrement des moisissures — Échantillonnage par impaction

⎯ Partie 19: Stratégie d'échantillonnage des moisissures

⎯ Partie 25: Détermination de l'émission de composés organiques semi-volatils des produits de

construction — Méthode de la micro-chambre
⎯ Partie 26: Stratégie de mesure du dioxyde de carbone (CO )

⎯ Partie 28: Évaluation sensorielle des émissions des matériaux et des produits de construction

Les parties suivantes sont prévues:

⎯ Partie 20: Détection et dénombrement des moisissures — Échantillonnage à partir de poussières

domestiques

⎯ Partie 21: Détection et dénombrement des moisissures — Échantillonnage à partir de matériaux

⎯ Partie 22: Détection et dénombrement des moisissures — Méthodes moléculaires

⎯ Partie 27: Méthode normalisée pour l'analyse quantitative des fibres d'amiante dans la poussière

En outre,
[2]

⎯ l'ISO 12219-1 (en préparation), Air intérieur — Véhicules routiers — Partie 1: Enceinte d'essai d'un

véhicule complet — Spécification et méthode de détermination des composés organiques volatils dans

les habitacles de voitures,
[3]

⎯ l'ISO 16017-1 , 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, et
[4]

⎯ l'ISO 16017-2 , 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 2: Échantillonnage par diffusion

traitent plus particulièrement des mesurages relatifs aux composés organiques volatils (COV).

© ISO 2008 – Tous droits réservés v
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ISO 16000-13:2008(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 l'échantillonnage de

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

dits (voir Avant-propos).

La présente partie de l'ISO 16000 s'applique au prélèvement des polychlorobiphényles (PCB) de type

dioxines, des polychlorodibenzo-p-dioxines (PCDD) et des polychlorodibenzofuranes (PCDF) dans l'air

intérieur, et à la préparation des supports d'échantillonnage requis pour l'échantillonnage. Les méthodes

d'échantillonnage décrites ici sont également applicables aux hydrocarbures aromatiques polycycliques (HAP)

à au moins deux cycles aromatiques. Les modes opératoires de préparation et d'extraction des supports

d'échantillonnage des HAP ainsi que de dosage analytique des HAP sont donnés dans l'ISO 12884 et sont,

par conséquent, exclus du présent document.

La stratégie d'échantillonnage pour l'analyse des PCB, des PCDD/PCDF et des HAP dans l'air intérieur est

décrite dans l'ISO 16000-12.

Plusieurs PCB et PCDD/PCDF sont considérés comme étant potentiellement cancérigènes pour l'Homme. Il

existe 209 PCB individuels (congénères), 75 PCDD et 135 PCDF. Les PCB les plus toxiques sont les PCB

coplanaires dont la structure est similaire à celle des PCDD. La PCDD la plus toxique est la

2,3,7,8-tétrachlorodibenzo-p-dioxine (2,3,7,8-TCDD).

Les PCB sont principalement émis dans l'air intérieur par les enduits extérieurs, certaines peintures et les

condensateurs électriques. Tous ont récemment été interdits. Les principales sources de PCDD/PCDF dans

l'air intérieur sont les impuretés des produits de préservation du bois, qui contiennent du pentachlorophénol

(PCP), et les émissions d'incendies impliquant des produits chlorés. Le sol amené des décharges et les

émissions issues de sites industriels abandonnés situés à proximité des bâtiments peuvent aussi contribuer à

la présence de PCB et de PCDD/PCDF dans l'environnement intérieur.

La concentration totale en PCB (six PCB marqueurs: PCB-28, -52, -101, -138, -153 et -180 multipliés par 5)

de l'air extérieur urbain est généralement comprise entre 10 et plusieurs centaines de picogrammes par mètre

cube (pg/m ). Dans l'air extérieur urbain, les PCDD/PCDF se trouvent habituellement à des concentrations

très faibles, par exemple de l'ordre du femtogramme par mètre cube (fg/m ) au picogramme par mètre cube

(pg/m ). Les PCB et les PCDD/PCDF peuvent être répartis entre les phases gazeuse et particulaire de l'air

ambiant ou de l'air intérieur, en fonction de la température, de l'humidité, du degré de chloration, de leur

concentration et de leur capacité à s'associer à la matière particulaire en suspension. Ces composés, en

particulier ceux dont la pression de vapeur est supérieure à 10 kPa, ont tendance à s'évaporer des filtres à

particules au cours de l'échantillonnage. Par conséquent, un piège adsorbant supplémentaire est présent

pour garantir l'efficacité de l'échantillonnage. L'analyse séparée du filtre et du piège adsorbant ne permet pas

d'obtenir la distribution des phases atmosphériques d'origine à température ambiante normale, en raison de la

volatilisation des composés du filtre. Par conséquent, il convient de ne pas réaliser ce type d'analyse.

L'expédition des étalons de PCDD/PCDF doit se conformer aux réglementations nationales. Ces composés

doivent être transportés dans des conteneurs spéciaux disponibles dans le commerce. Il convient de confier

leur manipulation uniquement à des opérateurs formés à cet effet.

La présente partie de l'ISO 16000 décrit l'échantillonnage des polychlorobiphényles (PCB) de type dioxines,

des polychlorodibenzo-p-dioxines (PCDD) et des polychlorodibenzofuranes (PCDF). L'extraction, la purification

et l'analyse sont décrits dans l'ISO 16000-14.
vi © ISO 2008 – Tous droits réservés
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NORME INTERNATIONALE ISO 16000-13:2008(F)
Air intérieur —
Partie 13:
Dosage des polychlorobiphényles (PCB) de type dioxine et des
polychlorodibenzo-p-dioxines
(PCDD)/polychlorodibenzofuranes (PCDF) totaux (en phase
gazeuse et en phase particulaire) — Collecte sur des filtres
adsorbants
1 Domaine d'application

La présente partie de l'ISO 16000 spécifie l'échantillonnage et la préparation des supports d'échantillonnage

des polychlorobiphényles (PCB) de type dioxine, des polychlorodibenzo-p-dioxines (PCDD) et des

polychlorodibenzofuranes (PCDF) dans l'air intérieur (voir Tableau C.1). La méthode intègre un mode

opératoire d'échantillonnage dans lequel les PCB et les PCDD/PCDF sont prélevés dans l'air sur un filtre à

fines particules muni d'un piège adsorbant. La méthode ne convient pas au dosage séparé des PCB et des

PCDD/PCDF gazeux et de ceux liés aux particules, car certains composés qui s'évaporent du filtre sont

recueillis par le piège adsorbant. La présente partie de l'ISO 16000 ne concerne pas les méthodes

analytiques relatives aux PCB, PCDD et PCDF qui sont traitées dans l'ISO 16000-14. (L'ISO 16000-13 et

l'ISO 16000-14 sont les deux parties qui traitent du mode opératoire général de mesure des PCB et des

PCDD/PCDF.)

Associée aux modes opératoires d'analyse spécifiés dans l'ISO 16000-14, qui inclut des analyses spécifiques

par chromatographie en phase gazeuse haute résolution et spectrométrie de masse haute résolution

(HRGC/HRMS), la présente méthode permet de détecter la plupart des PCB et des PCDF/PCDD à des

concentrations égales ou inférieures à 0,2 pg/m . Toutefois, il n'est pas toujours possible de détecter tous les

analytes présents à de telles concentrations, en particulier à de plus faibles débits d'échantillonnage. Pour

atteindre des limites de détection adéquates, il convient d'échantillonner au moins 50 m d'air. Pour des

opérations de mesurage normales, des volumes d'échantillonnage allant jusqu'à 360 m sont utilisés

3 3

(l'équivalent d'une période d'échantillonnage de 24 heures à 16 m /h ou de 7 jours à 2 m /h). La méthode a

été validée pour des périodes d'échantillonnage pouvant atteindre 7 jours. Avec des pièges adsorbants de

plus grande capacité, des volumes d'échantillonnage allant jusqu'à 1 000 m ont été validés.

La fidélité prévisible de l'échantillonnage dans des conditions normales peut atteindre ± 25 % ou plus et

l'incertitude ± 50 % ou plus.

Si les restrictions qui s'imposent sont appliquées, la présente méthode convient aux petites pièces, par

exemple les chambres d'enfants ou les bureaux.
© ISO 2008 – Tous droits réservés 1
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ISO 16000-13:2008(F)
2 Références normatives

Les documents de référence suivants sont indispensables pour l'application 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 12884, Air ambiant — Dosage des hydrocarbures aromatiques polycycliques totales (phase gazeuse et

particulaire) — Prélèvement sur filtres à sorption et analyses par chromatographie en phase

gazeuse/spectrométrie en masse

ISO 16000-12, Air intérieur — Partie 12: Stratégie d'échantillonnage des polychlorobiphényles (PCB), des

polychlorodibenzo-p-dioxines (PCDD), des polychlorodibenzofuranes (PCDF) et des hydrocarbures

aromatiques polycycliques (HAP)

ISO 16000-14, Air intérieur — Partie 14: Dosage des polychlorobiphényles (PCB) de type dioxine et des

polychlorodibenzo-p-dioxines (PCDD)/polychlorodibenzofuranes (PCDF) totaux (en phase gazeuse et en

phase particulaire) — Extraction, purification et analyse par chromatographie en phase gazeuse haute

résolution et spectrométrie de masse
3 Termes et définitions

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

3.1
efficacité de prélèvement
% E
capacité d'un échantillonneur à piéger et à retenir des composés cibles

NOTE Le % E est le pourcentage d'analyte cible recueilli et retenu par le support d'échantillonnage lors de

l'introduction dans l'échantillonneur d'air, lorsque l'échantillonneur fonctionne dans des conditions normales pendant une

durée supérieure ou égale à celle requise par l'usage prévu.
3.2
efficacité de rétention dynamique

capacité du support d'échantillonnage à retenir un PCB, un PCDD ou un PCDF donné qui a été ajouté dans le

piège adsorbant dans une solution de marquage, lorsque l'air est aspiré à travers l'échantillonneur dans des

conditions normales pendant une durée supérieure ou égale à celle requise par l'usage prévu

3.3
PCB de type dioxine

PCB non ortho et mono-ortho présentant une affinité pour le récepteur hydrocarbure aryle (Ah) et dont les

effets sont similaires à ceux des PCDD/PCDF substitués en positions 2, 3, 7, 8, d'après l'OMS

NOTE 1 Voir Référence [5].
NOTE 2 Voir également les Tableaux C.1 et C.2.
3.4
PCB marqueur
l'un des six PCB

NOTE Les six PCB marqueurs sont les PCB-28, PCB-52, PCB-101, PCB-138, PCB-153 et PCB–180.

2 © ISO 2008 – Tous droits réservés
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ISO 16000-13:2008(F)
3.5
marquage
ajout de PCB étalons marqués au C
3.6
caractéristique de fonctionnement opérationnelle

mesurage qui tient compte des effets de l'environnement physique et chimique et des problèmes d'entretien

EXEMPLE Tension du secteur, température, apport de certaines substances, temps de mise en place, période de

fonctionnement sans intervention (voir Référence [1]).
3.7
blanc de site

échantillon non exposé mais marqué du support d'échantillonnage [par exemple filtre, piège en mousse de

polyuréthanne (PUF) ou cartouche d'échantillonnage complète], amené sur le site et soumis à la totalité du

mode opératoire analytique, y compris l'extraction, la purification et l'identification

NOTE Cette valeur de mesurage est nécessaire pour assurer qu'il n'y a pas eu de contamination significative au

cours de l'ensemble des phases du processus de mesurage et pour vérifier que l'opérateur est capable d'effectuer une

quantification d'un niveau correspondant à l'étude.
3.8
blanc analytique

échantillon non exposé, mais marqué d'un réactif ou d'un support d'échantillonnage soumis à la totalité du

mode opératoire analytique, y compris l'extraction, la purification et l'identification

3.9
étalon de prélèvement

marqueur ajouté au support d'échantillonnage avant l'échantillonnage afin de déterminer l'efficacité globale de

la méthode
EXEMPLE PCB et PCDD/PCDF marqués au C .
3.10
étalon d'extraction

marqueur ajouté au support d'échantillonnage avant l'extraction qui sert au calcul des résultats

EXEMPLE PCB et PCDD/PCDF marqués au C .
3.11
congénère
substance qui appartient au groupe chimique des PCB, PCDD ou PCDF
NOTE Comprend les 209 PCB, les 75 PCDD et les 135 PCDF individuels.
3.12
isomère

PCB, PCDD ou PCDF de composition élémentaire identique, mais de structure différente

EXEMPLE Le 1-chlorobiphényle et le 2-chlorobiphényle sont des isomères.
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ISO 16000-13:2008(F)
4 Termes abrégés
(Voir également les Tableaux C.1 et C.2)
PCB polychlorobiphényles
PCDD polychlorodibenzo-p-dioxine
PCDF polychlorodibenzofurane
TeCB tétrachlorobiphényle
PeCB pentachlorobiphényle
HxCB hexachlorobiphényle
HpCB heptachlorobiphényle
TCDD tétrachlorodibenzo-p-dioxine
PeCDD pentachlorodibenzo-p-dioxine
HxCDD hexachlorodibenzo-p-dioxine
HpCDD heptachlorodibenzo-p-dioxine
OCDD octachlorodibenzo-p-dioxine
TCDF tétrachlorodibenzofurane
PeCDF pentachlorodibenzofurane
HxCDF hexachlorodibenzofurane
HpCDF heptachlorodibenzofurane
OCDF octachlorodibenzofurane
PTFE polytétrafluoroéthylène
5 Principe

Les PCB, les PCDD et les PCDF sont prélevés directement dans l'environnement intérieur par aspiration d'un

échantillon d'air à travers un filtre à fines particules muni d'un piège adsorbant en mousse de polyuréthanne

(PUF). Les composés peu volatils associés à la matière particulaire en suspension dans l'air sont

principalement prélevés sur le filtre à particules. Les composés gazeux qui passent à travers le filtre et les

composés qui s'évaporent du filtre sont recueillis par le piège en mousse de polyuréthanne.

La méthode est applicable aux pièces des habitations, des bureaux et des bâtiments publics ou commerciaux,

y compris ceux présentant de vastes espaces intérieurs (par exemple usines, entrepôts, stades fermés). Le

débit d'échantillonnage et le volume d'air prélevé dépendent de la taille de la pièce ou de l'espace intérieur

3 3

examinés. Le débit peut être compris entre 1,5 m /h et 16 m /h selon la tâche de mesurage.

Les supports d'échantillonnage (filtre et PUF) sont associés et extraits ensemble. Les modes opératoires

d'extraction sont normalement fondés sur l'extraction au Soxhlet à l'aide de toluène ou d'un solvant équivalent.

Les PCB/PCDD/PCDF étalons marqués au C sont ajoutés avant l'échantillonnage et l'extraction afin de

suivre l'efficacité de prélèvement et le rendement. Le marquage à l'aide de PCB/PCDD/PCDF marqués au

C avant échantillonnage est nécessaire à la détermination des taux de récupération des congénères de

PCB/PCDD/PCDF. Les pertes subies au cours de l'extraction et de la purification sont détectées et

compensées en utilisant ces substituts marqués par des isotopes comme étalons internes d'extraction pour la

quantification en même temps que les étalons de récupération ajoutés juste avant l'analyse par HRGC/HRMS.

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ISO 16000-13:2008(F)
6 Appareillage et matériels
6.1 Appareillage d'échantillonnage

Un dispositif d'échantillonnage type est schématiquement représenté à la Figure 1 et un module

d'échantillonnage type est représenté à la Figure 2.
Légende
1 module d'échantillonnage (voir Figure 2)
2 pompe de prélèvement de l'air
3 minuterie
4 régulateur de débit (avec électronique de mesure)
5 compteur de temps écoulé
Entrée d'air.
Évacuation.
Figure 1 — Schéma d'un dispositif d'échantillonnage type
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ISO 16000-13:2008(F)
a) Module d'échantillonnage type b) Vue en éclaté de l'assemblage
Légende
1 entrée d'air 8 grille de support du filtre
2 grille de support du filtre (identique à 8) 9 porte-filtre
3 module d'échantillonnage monté 10 cartouche adsorbante en verre (piège en PUF)
4 évacuation d'air 11 piège en PUF
5 pièce de retenue du filtre 12 porte-cartouche avec grille de support
6 joints d'étanchéité 13 porte-cartouche
7 filtre en fibre de quartz ou de verre

Figure 2 — Module d'échantillonnage type avec filtre à particules et piège en PUF

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ISO 16000-13:2008(F)

Le module d'échantillonnage représenté à la Figure 2 est la base de l'échantillonneur d'air extérieur utilisé

pour les hydrocarbures aromatiques polycycliques (HAP) décrit dans l'ISO 12884. Il repose sur un modèle

ayant fait l'objet d'une publication (Référence [6]) et sert également au dosage des PCDD et des PCDF dans

l'air ambiant (Référence [7]). Un module de ce type dont les dimensions sont celles du module décrit dans

3 3

l'ISO 12884 peut être utilisé pour des débits de prélèvement de 1,5 m /h à 16 m /h et des volumes totaux d'air

de 360 m , selon la capacité du dispositif d'échantillonnage d'air utilisé. Des modules de ce type, de

dimensions et de configurations diverses, peuvent être utilisés à condition d'être validés.

NOTE La vitesse de capture des particules d'un échantillonneur dépend de la vitesse frontale pendant

l'échantillonnage. Par exemple, d'après la loi de Stokes, il peut être estimé que l'aspiration d'air par un filtre de 100 mm à

3 3

un débit de 15 m /h prélève des particules inférieures à environ 40 µm. À un débit de prélèvement de 6 m /h, des

particules inférieures à environ 20 µm sont capturées. En réduisant de nouveau le débit de prélèvement à 1,5 m /h, des

particules inférieures à 10 µm à 12 µm sont recueillies. Pour les mesurages liés à l'air intérieur, l'expérience montre que

les différences de mesurage avec le même module d'échantillonnage à différents débits baissant jusqu'à 1,5 m /h sont

nulles ou négligeables. De même, l'utilisation d'une entrée sélective de fraction granulométrique (par exemple MP ou

2,5

MP ) a peu d'effet sur la teneur totale en PCB/PCDD/PCDF de l'échantillon, à moins qu'une source d'émissions de

composés associés à des particules ne se trouve à proximité.
3 3

De nombreux dispositifs d'échantillonnage peuvent fournir des débits d'air de 1,5 m /h à 16 m /h; certains

sont équipés de régulateurs de débit dont la plage de réglage est très grande, ce qui permet de sélectionner

le débit de prélèvement voulu. Les restrictions concernant les débits de prélèvement et les volumes d'air

prélevés autorisés sont abordées à l'Article 8. Des exemples de dispositifs d'échantillonnage sont présentés à

l'Annexe A.
6.2 Matériaux d'échantillonnage

6.2.1 Mousse de polyuréthanne, à alvéoles ouverts, de type polyéther, d'une masse volumique de

22 mg/cm , coupée en cylindres de 76 mm de longueur et de 62 mm de diamètre ou en d'autres dimensions

adaptées au module d'échantillonnage spécifiquement utilisé. Ils sont disponibles dans le commerce auprès

de plusieurs fournisseurs. Il convient que le diamètre des cylindres en PUF soit légèrement plus grand que le

diamètre intérieur de la cartouche adsorbante afin que l'air ne passe pas autour mais à travers les cylindres.

Le nettoyage est réalisé conformément à l'Article 7.

6.2.2 Filtre, en fibre de microquartz ou de verre, sans liant, rincé à l'acide, avec une efficacité de filtration

de 99,99 % en fraction massique ou plus pour les particules inférieures à 0,5 µm ou d'autre filtre de

dimensions adaptées au module d'échantillonnage spécifiquement utilisé. L'efficacité doit être certifiée par le

fournisseur du filtre.

6.2.3 Étalons de prélèvement marqués au C; pour la composition, se reporter aux Tableaux 1 et 2.

6.2.4 Papier d'aluminium, pour emballer les filtres et les pièges en PUF avant et après échantillonnage.

6.2
...

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