SIST ISO 16000-13:2013
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
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
ISO 16000-13:2008 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. 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. ISO 16000-13:2008 does not address analytical methods for PCBs, PCDDs and PCDFs, which are included in ISO 16000-14.
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 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. 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. L'ISO 16000‑13:2008 ne concerne pas les méthodes analytiques relatives aux PCB, PCDD et PCDF qui sont traitées 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
Standards Content (Sample)
SLOVENSKI STANDARD
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
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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 2008
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Published in Switzerland
ii © ISO 2008 – All rights reserved
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
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
⎯ 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.
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
−8
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
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 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
s
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
s
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
E
r
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
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
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
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
a
Air intake.
b
Exhaust.
Figure 1 — Schematic drawing of a typical sampling system
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
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).
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
pg
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
a
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
Table 2 — C -labelled PCBs congeners to be added to the sample at different stages of the
3 3
procedure for measurement of about 0,01 ng WHO-TEQ /m assuming 180 m of sampling volume
PCB
Total mass to be added before:
Solution: Sampling Extraction GC-Injection
a
(sampling standard) (extraction standard) (recovery standard)
Total volume in µl:
(e.g. in toluene, n-nonane) 100 100 at least 10
Congeners added Total mass
pg
C -2,3,4,4′-TeCB (60) 3 600
13 b
C -3,3′,4,5,5′-PeCB (127) 3 600
C -2,3,3′,4,5,5′-HxCB (159) 3 600
C -3,4,4′,5-TeCB (81) 3 600
C -3,3′,4,4′-TeCB (77) 3 600
C -3,3′,4,4′,5-PeCB (126) 3 600
C -3,3′,4,4′,5,5′-HxCB (169) 3 600
13 b
C -2,3,3′,4,4′-PeCB (105) 3 600
C -2,3,4,4′,5-PeCB (114) 3 600
C -2,3′,4,4′,5-PeCB (118) 3 600
C -2′,3,4,4′,5-PeCB (123) 3 600
C -2,3,3′,4,4′,5-HxCB (156) 3 600
C -2,3,3′,4,4′,5′-HxCB (157) 3 600
C -2,3′,4,4′,5,5′-HxCB (167) 3 600
C -2,3,3′,4,4′,5,5′-HpCB (189) 3 600
C -2,3′,4′,5-TeCB (70) 3 600
C -2,3,3′,5,5′-PeCB (111) 3 600
C -2,2′,3,3′,4,4′,5-HpCB (170) 3 600
a 13
Table 2 shows a selection of available C -labelled PCBs suitable as recovery standards. At least one shall be added for each
dioxin-like PCB containing fraction.
b
Attention should be paid to possible co-elution problems of PCB 127 and PCB 105 on certain commercially available columns
7 Preparation of sampling media
Heat the particle filters before use at 250 °C (glass) or at 400 °C (quartz) for 5 h, wrap them in
n-hexane-rinsed aluminium foil, and place them in clean, tightly-sealed containers (e.g. glass Petri dishes or
wide-mouth glass jars tightly sealed with PTFE tape) for storage and transport to and from the monitoring site.
Gently handle the filters with clean forceps.
Extract PUF cylinders for 24 h with acetone in a Soxhlet extractor at approximately 4 cycles/h, then for
another 24 h with toluene in a Soxhlet extractor at approximately 4 cycles/h, and afterwards conduct a short
extraction with pentane for easy drying. Dry in a desiccator under vacuum and a gentle stream of high-purity
nitrogen or in a vacuum drying cabinet at 40 °C.
The extract from the Soxhlet extraction procedure from each batch may be analysed to determine initial
cleanliness prior to certification.
For storage, place the cleaned PUF plug in n-hexane-rinsed aluminium foil. For sampling preparation, the
PUF plug is placed into the glass sampling cartridge using polyester or latex rubber gloves and PTFE-coated
forceps. The sampling cartridge is wrapped with n-hexane-rinsed aluminium foil, placed in a clean container,
and tightly sealed for storage and transport to and from the monitoring site.
If desired, the loaded glass sampling cartridge and filter may be placed in the sampling module, which is in
turn placed in a clean container, and tightly sealed for storage and transport to and from the monitoring site.
The PUF cylinders may be reused if properly cleaned with toluene after each use. The number of possible
uses before significant deterioration of performance occurs has not been determined, but it should not be
used more than six times without verifying that the performance is unchanged.
8 Sampling
Before sampling, the boundary conditions to be taken into account shall be defined and noted as described in
ISO 16000-12.
Choose a suitable pumping system and sampling module according to the measurement task (see Annex A).
The hourly air flow rate of the sampling apparatus should not exceed 10 % of the air change rate of the room
in question. If the air change rate is unknown, the air volume sampled per hour shall not exceed 10 % of the
volume of the room. Low-volume sampling can be used for small rooms, for example children’s rooms.
High-volume sampling may be considered for very large indoor areas if the noise produced by the sampler is
of no consequence, provided that the constraints on sampling rate or air volume specified above are observed.
Conduct a leak check before and after sampling (see Clause 9). Plug the nozzle and evacuate the sampling
module to the minimum pressure used during sampling: the volume flow rate shall be less than 5 % of the
normal flow rate.
Take a field blank before each sampling campaign.
Confirm the efficiency of the sampler for the targeted PCBs/PCDDs/PCDFs under the conditions anticipated in
the field prior to the initiation of any sampling programme. Determination of the efficiency is particularly
important if sampling periods exceeding 24 h are planned. Acceptable performance may be established by
determining sampling efficiency, E , directly or estimating it from the dynamic retention efficiency, E . Refer to
s r
Annex B for instructions on determining sampling efficiency.
When the sampling module is being loaded with particle filter and PUF trap, take special care to ensure that
there is no contamination, e.g. by skin oils (use gloves and forceps). Take special care that PUF trap is seated
properly in the module, and that channels and cavities do not form. Carefully seal the sampling module
(e.g. with PTFE tape) to ensure that it is leak-proof.
Before placing the particle filter holder [see part 9 in Figure 2 b)] on the sampling module, use a micro-litre
syringe to spike the surface of inlet face of the PUF sorbent with 50 pg each of C -1,2,3,7,8-PeCDF,
13 13 13
C -1,2,3,7,8,9-HxCDF and 100 pg of C -1,2,3,4,7,8,9-HpCDF as well as C -2,3,4,4′-TeCB,
12 12 12
13 13
C -3,3′,4,5,5′-PeCB and C -2,3,3′,4,5,5′-HxCB all in 100 µl of toluene containing 4 % n-tetradecane as
12 12
keeper, and keep it cool before use. The spiking standard can also be added to the PUF sorbent in the
laboratory shortly before sampling is performed (not more than 24 h before sampling), provided that the PUF
media are kept refrigerated to minimize losses prior to sampling. This procedure may avoid contamination on
site and safety issue that may prohibit application on site.
Monitor the airflow through the sampling system monitored by a flow-control device or devices. Conduct a
multi-point calibration of the flow-control system every six months using a standard audit calibration orifice,
which is temporarily attached to the inlet of the sampler. Alternatively, use a high-flow dry gas metre if it has
been validated as a transfer standard.
10 © ISO 2008 – All rights reserved
The sampler shall be calibrated:
a) when new;
b) after major repairs or maintenance;
c) whenever any audit point deviates from the calibration curve by more than 7 %; or
d) at the frequency specified in the user’s manual.
Calibration and re-calibration of the gas meter in the field is performed according to laboratory quality
standards, e.g. using a calibrated orifice flow rate transfer standard.
Under the unlikely conditions of very high airborne dust loadings, the air flow rate through the filter can
decrease markedly during the course of sampling, especially if the flow rate is not automatically controlled.
Even with flow-controlled pumps, the filter load can become so high that the apparatus may switch off
automatically. Therefore, the filter should be changed if the air flow rate changes by more than 10 % of the
initial value. The new filter shall also be spiked with the sampling standards.
If it is desired to correct the sampling volume to standard conditions of pressure and temperature
(1 013,25 hPa; 273,15 K), use the mean temperature and mean air pressure measured during sampling.
Take special care that the sampling system is installed so that it is not directly influenced by draughts, etc. To
ensure representative sampling, take care that the air change rate in the room during the sampling period is
similar to that during normal use of the room. To minimize a possible noise nuisance due to the sampling
apparatus, it can be installed in a side room or outdoors. In this case, connect the sampling module to the
pumping system unit using a tube connection (e.g. PVC tubular fabric) via a hose connector. Note, however,
that the longer the tubing, the greater the pressure drop and burden placed on the pumping system. Smaller
pumping systems may be silenced by placing them in polyurethane or polystyrene containers such as ice
chests. However, care should be exercised that the systems do not overheat.
To determine a representative average value of the PCB/PCDD/PCDF concentrations in air, it may be
necessary to carry out sampling over relatively long periods. For normal measurement, tasks sampling
3 3 3
volumes shall not exceed 360 m (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. In special cases sampling volumes of
high-volume samplers up to 1 000 m are validated.
After sampling, record the sampling duration, wrap the sampling module in aluminium foil and keep it cool until
it is returned to the laboratory. The filter and PUF trap should be removed from the sampling module in the
laboratory and placed in tightly-sealed glass or metal containers and stored at 4 °C or lower temperatures until
analysis. Keep the storage time as short as possible, in no case longer than two weeks. Alternatively, if
special care is taken to avoid contamination, the PUF cartridge and filter may be removed from the sampling
module and placed into the storage containers at the sampling site.
Sampling periods in excess of 24 h should be avoided unless necessary to achieve the necessary limit of
detection. Rather than prolonging the sampling period, the use of a sampler with a higher sampling rate
should be considered, provided that its use will not upset the ventilation rate of the room or interior space
being monitored or present an unacceptably intrusive situation with respect to noise production or space
consumption. Modification of the determinative steps, such as carefully increasing concentration of the extract
or using more sensitive MS techniques, may also enable lower detection limits.
Extraction, clean-up and analytical procedures are described in ISO 16000-14.
9 Minimum requirements for sampling
The following minimum requirements shall be fulfilled for the determination of PCB/PCDD/PCDF
concentrations.
a) A leak check shall be carried out before and after every sampling procedure. The sampling module with
its intake sealed shall be evacuated to the pressure used during sampling and the volume flow rate shall
be less than 5 % of the normal flow rate.
b) A field blank shall be taken before each sampling campaign.
c) The C -labelled standards shall be used as described in Tables 1 and 2.
d) The sampling standard solution shall contain 4 % tetradecane as a keeper.
e) The recovery rate for each sampling standard shall be greater than 50 % calculated on the basis of the
relevant extraction standard.
f) The PCB/PCDD/PCDF concentrations in the field blank shall be more than a factor of 5 below the lowest
measurement values (expressed in TEQ) assuming the same volume as for sampling. If the calculated
value measured is less than the preceding field blank value, the reported result is defined as less than or
equal to the blank.
12 © ISO 2008 – All rights reserved
Annex A
(informative)
Details of samplers
A.1 General
Examples of several sampling systems that may be used to efficiently collect PCBs, PCDDs and PCDFs from
indoor air are presented in this annex. All of these samplers are based on the principles described in Clause 5
and in 6.1. The sampling media in all cases consist of a glass- or quartz-fibre particle filter backed up by a
PUF trap. In each case, the PUF traps are held in cylindrical glass or stainless steel sampling cartridges.
The diameter of the PUF plug should be about 2 mm to 5 mm larger than the internal diameter of the cartridge
so that it is slightly compressed. If uncompressed, air may flow between the glass cylinder walls of the
cartridge and the PUF, resulting in sampling errors. This can be easily done without compressing the foam
lengthwise if the foam is pushed into the cylinder, then pulled back slightly.
When available, particle size-selective inlets (e.g. PM or PM ), may be used if desired.
2,5 10
The user may substitute other samplers but shall meet the requirements of this part of ISO 16000.
A.2 Low-volume samplers
A.2.1 US EPA method IP-7 low-volume sampler
3 3
The sampler shown in Figure A.1 is designed to operate at 1,2 m /h to 1,6 m /h and is quiet enough for use in
occupied dwellings and offices. The sampler consists of an air pump and associated controls housed in an
acoustically-insulated compartment and connected by way of a hose to a sampling module that holds a
circular glass- or quartz-fibre filter backed by a glass sorbent cartridge containing a cylindrical PUF plug (see
Figure A.2). It is described in References [8] and [9].
Any pump pr
...
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 2008
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Published in Switzerland
ii © ISO 2008 – All rights reserved
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
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
⎯ 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.
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
−8
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
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 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
s
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
s
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
E
r
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
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
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
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
a
Air intake.
b
Exhaust.
Figure 1 — Schematic drawing of a typical sampling system
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
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).
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
pg
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
a
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
Table 2 — C -labelled PCBs congeners to be added to the sample at different stages of the
3 3
procedure for measurement of about 0,01 ng WHO-TEQ /m assuming 180 m of sampling volume
PCB
Total mass to be added before:
Solution: Sampling Extraction GC-Injection
a
(sampling standard) (extraction standard) (recovery standard)
Total volume in µl:
(e.g. in toluene, n-nonane) 100 100 at least 10
Congeners added Total mass
pg
C -2,3,4,4′-TeCB (60) 3 600
13 b
C -3,3′,4,5,5′-PeCB (127) 3 600
C -2,3,3′,4,5,5′-HxCB (159) 3 600
C -3,4,4′,5-TeCB (81) 3 600
C -3,3′,4,4′-TeCB (77) 3 600
C -3,3′,4,4′,5-PeCB (126) 3 600
C -3,3′,4,4′,5,5′-HxCB (169) 3 600
13 b
C -2,3,3′,4,4′-PeCB (105) 3 600
C -2,3,4,4′,5-PeCB (114) 3 600
C -2,3′,4,4′,5-PeCB (118) 3 600
C -2′,3,4,4′,5-PeCB (123) 3 600
C -2,3,3′,4,4′,5-HxCB (156) 3 600
C -2,3,3′,4,4′,5′-HxCB (157) 3 600
C -2,3′,4,4′,5,5′-HxCB (167) 3 600
C -2,3,3′,4,4′,5,5′-HpCB (189) 3 600
C -2,3′,4′,5-TeCB (70) 3 600
C -2,3,3′,5,5′-PeCB (111) 3 600
C -2,2′,3,3′,4,4′,5-HpCB (170) 3 600
a 13
Table 2 shows a selection of available C -labelled PCBs suitable as recovery standards. At least one shall be added for each
dioxin-like PCB containing fraction.
b
Attention should be paid to possible co-elution problems of PCB 127 and PCB 105 on certain commercially available columns
7 Preparation of sampling media
Heat the particle filters before use at 250 °C (glass) or at 400 °C (quartz) for 5 h, wrap them in
n-hexane-rinsed aluminium foil, and place them in clean, tightly-sealed containers (e.g. glass Petri dishes or
wide-mouth glass jars tightly sealed with PTFE tape) for storage and transport to and from the monitoring site.
Gently handle the filters with clean forceps.
Extract PUF cylinders for 24 h with acetone in a Soxhlet extractor at approximately 4 cycles/h, then for
another 24 h with toluene in a Soxhlet extractor at approximately 4 cycles/h, and afterwards conduct a short
extraction with pentane for easy drying. Dry in a desiccator under vacuum and a gentle stream of high-purity
nitrogen or in a vacuum drying cabinet at 40 °C.
The extract from the Soxhlet extraction procedure from each batch may be analysed to determine initial
cleanliness prior to certification.
For storage, place the cleaned PUF plug in n-hexane-rinsed aluminium foil. For sampling preparation, the
PUF plug is placed into the glass sampling cartridge using polyester or latex rubber gloves and PTFE-coated
forceps. The sampling cartridge is wrapped with n-hexane-rinsed aluminium foil, placed in a clean container,
and tightly sealed for storage and transport to and from the monitoring site.
If desired, the loaded glass sampling cartridge and filter may be placed in the sampling module, which is in
turn placed in a clean container, and tightly sealed for storage and transport to and from the monitoring site.
The PUF cylinders may be reused if properly cleaned with toluene after each use. The number of possible
uses before significant deterioration of performance occurs has not been determined, but it should not be
used more than six times without verifying that the performance is unchanged.
8 Sampling
Before sampling, the boundary conditions to be taken into account shall be defined and noted as described in
ISO 16000-12.
Choose a suitable pumping system and sampling module according to the measurement task (see Annex A).
The hourly air flow rate of the sampling apparatus should not exceed 10 % of the air change rate of the room
in question. If the air change rate is unknown, the air volume sampled per hour shall not exceed 10 % of the
volume of the room. Low-volume sampling can be used for small rooms, for example children’s rooms.
High-volume sampling may be considered for very large indoor areas if the noise produced by the sampler is
of no consequence, provided that the constraints on sampling rate or air volume specified above are observed.
Conduct a leak check before and after sampling (see Clause 9). Plug the nozzle and evacuate the sampling
module to the minimum pressure used during sampling: the volume flow rate shall be less than 5 % of the
normal flow rate.
Take a field blank before each sampling campaign.
Confirm the efficiency of the sampler for the targeted PCBs/PCDDs/PCDFs under the conditions anticipated in
the field prior to the initiation of any sampling programme. Determination of the efficiency is particularly
important if sampling periods exceeding 24 h are planned. Acceptable performance may be established by
determining sampling efficiency, E , directly or estimating it from the dynamic retention efficiency, E . Refer to
s r
Annex B for instructions on determining sampling efficiency.
When the sampling module is being loaded with particle filter and PUF trap, take special care to ensure that
there is no contamination, e.g. by skin oils (use gloves and forceps). Take special care that PUF trap is seated
properly in the module, and that channels and cavities do not form. Carefully seal the sampling module
(e.g. with PTFE tape) to ensure that it is leak-proof.
Before placing the particle filter holder [see part 9 in Figure 2 b)] on the sampling module, use a micro-litre
syringe to spike the surface of inlet face of the PUF sorbent with 50 pg each of C -1,2,3,7,8-PeCDF,
13 13 13
C -1,2,3,7,8,9-HxCDF and 100 pg of C -1,2,3,4,7,8,9-HpCDF as well as C -2,3,4,4′-TeCB,
12 12 12
13 13
C -3,3′,4,5,5′-PeCB and C -2,3,3′,4,5,5′-HxCB all in 100 µl of toluene containing 4 % n-tetradecane as
12 12
keeper, and keep it cool before use. The spiking standard can also be added to the PUF sorbent in the
laboratory shortly before sampling is performed (not more than 24 h before sampling), provided that the PUF
media are kept refrigerated to minimize losses prior to sampling. This procedure may avoid contamination on
site and safety issue that may prohibit application on site.
Monitor the airflow through the sampling system monitored by a flow-control device or devices. Conduct a
multi-point calibration of the flow-control system every six months using a standard audit calibration orifice,
which is temporarily attached to the inlet of the sampler. Alternatively, use a high-flow dry gas metre if it has
been validated as a transfer standard.
10 © ISO 2008 – All rights reserved
The sampler shall be calibrated:
a) when new;
b) after major repairs or maintenance;
c) whenever any audit point deviates from the calibration curve by more than 7 %; or
d) at the frequency specified in the user’s manual.
Calibration and re-calibration of the gas meter in the field is performed according to laboratory quality
standards, e.g. using a calibrated orifice flow rate transfer standard.
Under the unlikely conditions of very high airborne dust loadings, the air flow rate through the filter can
decrease markedly during the course of sampling, especially if the flow rate is not automatically controlled.
Even with flow-controlled pumps, the filter load can become so high that the apparatus may switch off
automatically. Therefore, the filter should be changed if the air flow rate changes by more than 10 % of the
initial value. The new filter shall also be spiked with the sampling standards.
If it is desired to correct the sampling volume to standard conditions of pressure and temperature
(1 013,25 hPa; 273,15 K), use the mean temperature and mean air pressure measured during sampling.
Take special care that the sampling system is installed so that it is not directly influenced by draughts, etc. To
ensure representative sampling, take care that the air change rate in the room during the sampling period is
similar to that during normal use of the room. To minimize a possible noise nuisance due to the sampling
apparatus, it can be installed in a side room or outdoors. In this case, connect the sampling module to the
pumping system unit using a tube connection (e.g. PVC tubular fabric) via a hose connector. Note, however,
that the longer the tubing, the greater the pressure drop and burden placed on the pumping system. Smaller
pumping systems may be silenced by placing them in polyurethane or polystyrene containers such as ice
chests. However, care should be exercised that the systems do not overheat.
To determine a representative average value of the PCB/PCDD/PCDF concentrations in air, it may be
necessary to carry out sampling over relatively long periods. For normal measurement, tasks sampling
3 3 3
volumes shall not exceed 360 m (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. In special cases sampling volumes of
high-volume samplers up to 1 000 m are validated.
After sampling, record the sampling duration, wrap the sampling module in aluminium foil and keep it cool until
it is returned to the laboratory. The filter and PUF trap should be removed from the sampling module in the
laboratory and placed in tightly-sealed glass or metal containers and stored at 4 °C or lower temperatures until
analysis. Keep the storage time as short as possible, in no case longer than two weeks. Alternatively, if
special care is taken to avoid contamination, the PUF cartridge and filter may be removed from the sampling
module and placed into the storage containers at the sampling site.
Sampling periods in excess of 24 h should be avoided unless necessary to achieve the necessary limit of
detection. Rather than prolonging the sampling period, the use of a sampler with a higher sampling rate
should be considered, provided that its use will not upset the ventilation rate of the room or interior space
being monitored or present an unacceptably intrusive situation with respect to noise production or space
consumption. Modification of the determinative steps, such as carefully increasing concentration of the extract
or using more sensitive MS techniques, may also enable lower detection limits.
Extraction, clean-up and analytical procedures are described in ISO 16000-14.
9 Minimum requirements for sampling
The following minimum requirements shall be fulfilled for the determination of PCB/PCDD/PCDF
concentrations.
a) A leak check shall be carried out before and after every sampling procedure. The sampling module with
its intake sealed shall be evacuated to the pressure used during sampling and the volume flow rate shall
be less than 5 % of the normal flow rate.
b) A field blank shall be taken before each sampling campaign.
c) The C -labelled standards shall be used as described in Tables 1 and 2.
d) The sampling standard solution shall contain 4 % tetradecane as a keeper.
e) The recovery rate for each sampling standard shall be greater than 50 % calculated on the basis of the
relevant extraction standard.
f) The PCB/PCDD/PCDF concentrations in the field blank shall be more than a factor of 5 below the lowest
measurement values (expressed in TEQ) assuming the same volume as for sampling. If the calculated
value measured is less than the preceding field blank value, the reported result is defined as less than or
equal to the blank.
12 © ISO 2008 – All rights reserved
Annex A
(informative)
Details of samplers
A.1 General
Examples of several sampling systems that may be used to efficiently collect PCBs, PCDDs and PCDFs from
indoor air are presented in this annex. All of these samplers are based on the principles described in Clause 5
and in 6.1. The sampling media in all cases consist of a glass- or quartz-fibre particle filter backed up by a
PUF trap. In each case, the PUF traps are held in cylindrical glass or stainless steel sampling cartridges.
The diameter of the PUF plug should be about 2 mm to 5 mm larger than the internal diameter of the cartridge
so that it is slightly compressed. If uncompressed, air may flow between the glass cylinder walls of the
cartridge and the PUF, resulting in sampling errors. This can be easily done without compressing the foam
lengthwise if the foam is pushed into the cylinder, then pulled back slightly.
When available, particle size-selective inlets (e.g. PM or PM ), may be used if desired.
2,5 10
The user may substitute other samplers but shall meet the requirements of this part of ISO 16000.
A.2 Low-volume samplers
A.2.1 US EPA method IP-7 low-volume sampler
3 3
The sampler shown in Figure A.1 is designed to operate at 1,2 m /h to 1,6 m /h and is quiet enough for use in
occupied dwellings and offices. The sampler consists of an air pump and associated controls housed in an
acoustically-insulated compartment and connected by way of a hose to a sampling module that holds a
circular glass- or quartz-fibre filter backed by a glass sorbent cartridge containing a cylindrical PUF plug (see
Figure A.2). It is described in References [8] and [9].
Any pump providing the prescribed air flow rate may be used, but it shall be sound-insulated for use in
occupied dwellings or offices. When operated at 1,2 m /h, the pumping system described in References [7]
and [8] meets preferred noise criterion (PNC) 39 dB (less than 45 dB) (see Reference [10]), which is typical of
background noise in living areas and private offices. However, other commercially available air sampling
3 3
pumps that are capable of sampling at 1,2 m /h to 1,6 m /h are nearly as quiet, and noisier pumps may be
quieted by placing them in sound-insulated boxes such as polystyrene foam coolers provided that they do not
overheat.
Sampling periods of up to seven days may be required to collect sufficient samples to quantify low levels of
PCBs, PCDDs, and PCDFs in indoor air.
Key
1 sampling module (see Figure A.2)
2 pumping unit in acoustically-insulated box, 51 cm × 35 cm × 21 cm
3 sample hose line
4 dust cover
5 portable filter support screen
6 fibreglass acoustic insulation
7 holder
8 vacuum pump
9 flow transducer
10 fan
11 vents
12 electronic controls for flow control, etc.
13 seven-day programmable timer
Figure A.1 — Low-volume indoor air sampler with acoustic enclosure
14 © ISO 2008 – All rights reserved
Key
1 aluminium sampling module, cylinder, 64 mm ∅ outer (47 mm ∅ inner) × 145 mm long, with screw-on filter retainer
2 glass cartridge for PUF sorbent, cyl
...
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 2008
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Publié en Suisse
ii © ISO 2008 – Tous droits réservés
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
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
⎯ 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).
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
−8
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
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.
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
s
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
s
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
E
r
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
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.
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.
4 © ISO 2008 – Tous droits réservés
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
a
Entrée d'air.
b
Évacuation.
Figure 1 — Schéma d'un dispositif d'échantillonnage type
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
6 © ISO 2008 – Tous droits réservés
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.
6.2.5 Pince et gants en latex ou néoprène, pour manipuler le filtre et les pièges en PUF.
6.2.6 Micropipette, pour appliquer les étalons de récupération sur le filtre.
6.2.7 Ruban en PTFE, pour sceller hermétiquement le tube d'aspiration dans la douille à pas de vis du
boîtier de protection.
6.2.8 Bocal en verre ou autre récipient adapté, hermétique, pour stocker et transporter les pièges en
PUF et les filtres à particules.
6.2.9 Dessiccateur ou armoire de séchage sous vide.
6.2.10 Pompe à membrane ou autre pompe adaptée.
6.3 Réactifs analytiques
6.3.1 Toluène, distillé sur verre, de qualité chromatographique ou «pesticide».
6.3.2 n-hexane, distillé sur verre, de qualité chromatographique ou «pesticide».
6.3.3 Dichlorométhane, distillé sur verre, de qualité chromatographique ou «pesticide».
6.3.4 Acétone, distillé sur verre, de qualité chromatographique ou «pesticide».
6.3.5 n-nonane, distillé sur verre, de qualité chromatographique ou «pesticide».
6.3.6 n-tétradécane (solvant de garde), distillé sur verre, de qualité chromatographique ou «pesticide».
6.3.7 Étalons d'extraction marqués au C , pour la composition, se reporter aux Tableaux 1 et 2
(voir 6.4).
6.3.8 Étalons d'injection marqués au C , pour la composition, se reporter aux Tableaux 1 et 2
(voir 6.4).
6.4 Étalons marqués au C
Les masses des étalons de prélèvement marqués au C dans 100 µl de solvant adéquat (par exemple
toluène ou n-tétradécane/n-nonane à 4 %) qu'il convient d'ajouter à chaque échantillon à un niveau de
3 3
concentration d'environ 100 fg de TEQ/m pour un volume prélevé d'environ 180 m sont indiquées dans le
Tableau 1 (PCDD/PCDF) et le Tableau 2 (PCB). Pour les TEQ et les TEQ -OMS, voir Article C.3.
PCB
Il convient d'ajouter les étalons d'extraction aux différents supports d'échantillonnage dès la réception des
échantillons par le laboratoire. Les congénères marqués au C sont utilisés pour la quantification, car leur
comportement à la purification est exactement le même que celui des PCB, PCDD et PCDF extraits natifs en
raison de leurs propriétés chimiques et physiques quasiment identiques. Les étalons d'injection (voir
Tableau 1) servent à déterminer les taux de récupération. Si des masses de PCB, PCDD ou PCDF natifs
nettement supérieures sont attendues dans l'échantillon, les masses des étalons à utiliser spécifiées dans le
Tableau 1 et le Tableau 2 doivent être ajustées en conséquence. L'utilisation et la manipulation des étalons
d'extraction et de récupération sont décrites dans l'ISO 16000-14.
8 © ISO 2008 – Tous droits réservés
Tableau 1 — Congénères de 2,3,7,8-PCDD/PCDF marqués au C à ajouter aux échantillons avant
prélèvement, extraction et injection dans le chromatographe pour un niveau d'environ 100 fg TEQ/m
et un volume prélevé d'environ 180 m
Solution à ajouter avant:
Solution: Échantillonnage Extraction Injection dans le
(étalon de prélèvement) (étalon d'extraction) chromatographe
Volume total en µl:
(étalon de récupération)
(par exemple, dans le toluène
ou le n-nonane) 100 100 25
Congénères ajoutés Masse totale
pg
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-HpCDF 50
13 a
C -1,2,3,4,6,7,8-HpCDD 50
C -OCDF 50
C -OCDD 50
a
Ces étalons servent à quantifier les congénères restants des groupes d'homologues chlorés associés pour lesquels aucun étalon
n'a été ajouté.
Tableau 2 — Congénères de PCB marqués au C à ajouter à l'échantillon à différentes étapes du
mode opératoire pour le mesurage d'un niveau d'environ 0,01 ng TEQ -OMS/m et un volume
PCB
prélevé estimé à 180 m
Masse totale à ajouter avant:
Solution: Échantillonnage Extraction Injection dans le
(étalon de prélèvement) (étalon d'extraction) chromatographe
Volume total en µl:
a
(étalon de récupération)
(par exemple, dans le toluène
ou le n-nonane)
100 100 au moins 10
Congénères ajoutés Masse totale
pg
C -2,3,4,4′-TeCB (60) 3 600
13 b
C -3,3′,4,5,5′-PeCB (127) 3 600
C -2,3,3′,4,5,5′-HxCB (159) 3 600
C -3,4,4′,5-TeCB (81) 3 600
C -3,3′,4,4′-TeCB (77) 3 600
C -3,3′,4,4′,5-PeCB (126) 3 600
C -3,3′,4,4′,5,5′HxCB (169) 3 600
13 b
C -2,3,3′,4,4′-PeCB (105) 3 600
C -2,3,4,4′,5-PeCB (114) 3 600
C -2,3′,4,4′,5-PeCB (118) 3 600
C -2′,3,4,4′,5-PeCB (123) 3 600
C -2,3,3′,4,4′,5-HxCB (156) 3 600
C -2,3,3′,4,4′,5′-HxCB (157) 3 600
C -2,3′,4,4′,5,5′-HxCB (167) 3 600
C -2,3,3′,4,4′,5,5′-HpCB (189) 3 600
C -2,3′,4′,5-TeCB (70) 3 600
C -2,3,3′,5,5′-PeCB (111) 3 600
C -2,2′,3,3′,4,4′,5-HpCB (170) 3 600
a 13
Le Tableau 2 présente une sélection des PCB marqués au C disponibles comme étalons de récupération. Au moins l'un
d'entre eux doit être ajouté à chaque fraction contenant un PCB de type dioxine.
b
Il convient de surveiller l'apparition éventuelle de problèmes de coélution des PCB 127 et PCB 105 sur certaines colonnes
disponibles dans le commerce.
7 Préparation des supports d'échantillonnage
Avant utilisation, chauffer les filtres à particules à 250 °C (pour le verre) ou à 400 °C (pour le quartz) pendant
5 h, les envelopper dans du papier d'aluminium rincé au n-hexane et les placer dans des récipients
hermétiquement clos et propres (par exemple boîtes de Pétri en verre ou bocaux en verre à large ouverture
dont l'étanchéité est assurée par du ruban en PTFE) pour le stockage et le transport vers et en provenance
du site examiné. Manipuler les filtres avec précaution à l'aide d'une pince propre.
Extraire les cylindres en PUF pendant 24 h à l'acétone dans un extracteur Soxhlet à un rythme d'environ
4 cycles/h, puis de nouveau pendant 24 h au toluène dans un extracteur Soxhlet à environ 4 cycles/h et enfin
effectuer une extraction rapide au pentane pour un séchage rapide. Sécher dans un dessiccateur sous vide
sous courant léger d'azote de pureté élevée ou dans une armoire de séchage sous vide à 40 °C.
L'extrait obtenu par extraction au Soxhlet de chaque lot peut être analysé afin de déterminer la propreté
initiale avant certification.
10 © ISO 2008 – Tous droits réservés
Pour le stockage, placer le tampon PUF propre dans du papier d'aluminium rincé au n-hexane. Pour la
préparation de l'échantillonnage, le tampon PUF est placé dans la cartouche d'échantillonnage en verre à
l'aide de gants en polyester ou en caoutchouc de latex et d'une pince revêtue de PTFE. Envelopper la
cartouche d'échantillonnage dans du papier d'aluminium rincé au n-hexane, la placer dans un récipient propre
et fermer celui-ci hermétiquement pour le stockage et le transport vers et en provenance du site examiné.
Il est possible de placer la cartouche d'échantillonnage en verre chargée dans le module d'échantillonnage,
qui est lui-même placé dans un récipient propre, fermé hermétiquement pour le stockage et le transport vers
et en provenance du site examiné.
Les cylindres en PUF sont réutilisables à condition d'être nettoyés avec soin au toluène après chaque
utilisation. Le nombre d'utilisations possibles avant une détérioration notable des performances n'a pas été
déterminé, mais il convient de ne pas utiliser un cylindre plus de six fois sans vérifier l'intégrité des
performances.
8 Échantillonnage
Avant l'échantillonnage, les conditions limites à prendre en compte doivent être définies et notées, comme
cela est décrit dans l'ISO 16000-12.
Choisir un système de pompage approprié et un module d'échantillonnage en fonction de l'opération de
mesurage (voir Annexe A). Il convient que le débit d'air horaire du dispositif d'échantillonnage ne dépasse pas
10 % du taux de renouvellement de l'air dans la pièce en question. Si le taux de renouvellement de l'air est
inconnu, le volume d'air prélevé par heure ne doit pas dépasser 10 % du volume de la pièce. Un
échantillonnage de faible volume peut être réalisé dans les petites pièces telles que les chambres d'enfant.
Un échantillonnage de grand volume peut être envisagé pour les très grands espaces intérieurs à condition
que le bruit émis par l'échantillonneur soit sans conséquence et que les contraintes de débit d'échantillonnage
et de volume d'air spécifiées ci-dessus soient respectées. Effectuer un contrôle d'étanchéité avant et après
échantillonnage (voir Article 9). Boucher la buse d'aspiration et mettre la ligne de prélèvement à la pression
minimale appliquée pendant le prélèvement: le débit de fuite doit être inférieur à 5 % du débit normal.
Effectuer un blanc de site avant chaque série d'échantillonnage.
Confirmer l'efficacité de l'échantillonneur vis-à-vis des PCB, PCDD et PCDF cibles dans les conditions
prévues sur site avant de démarrer le programme d'échantillonnage. La détermination de l'efficacité est
particulièrement importante si des périodes d'échantillonnage supérieures à 24 h sont prévues. Une
performance acceptable peut être établie en déterminant l'efficacité de prélèvement, E , directement ou en la
s
déduisant de l'efficacité de rétention dynamique, E . Se reporter à l'Annexe B pour les instructions relatives à
r
la détermination de l'efficacité de prélèvement.
Lors du chargement du module d'échantillonnage avec filtre à particules et piège en PUF, veiller à éviter toute
contamination, par exemple par les substances grasses de la peau (utiliser des gants et une pince). Veiller à
ce que le piège en PUF soit correctement introduit dans le module et qu'aucun canal ni aucune cavité ne se
forme. Rendre étanche le module d'échantillonnage (par exemple à l'aide de ruban en PTFE) pour garantir
l'absence de fuite.
Avant de placer le porte-filtre à particules [voir partie 9 à la Figure 2 b)] sur le module d'échantillonnage,
marquer la surface de l'adsorbant en PUF côté entrée d'air à l'aide d'une micropipette avec 50 pg de
13 13 13
C -1,2,3,7,8-PeCDF, 50 pg de C -1,2,3,7,8,9-HxCDF et 100 pg de C -1,2,3,4,7,8,9-HpCDF, 100 pg
12 12 12
13 13 13
de C -2,3,4,4′-TeCB, 100 pg de C -3,3′,4,5,5′-PeCB et 100 pg de C -2,3,3′,4,5,5′-HxCB, chacun
12 12 12
dans 100 µl de toluène contenant 4 % de n-tétradécane comme solvant de garde et maintenir au frais avant
utilisation. L'étalon de marquage peut également être ajouté à l'adsorbant en PUF dans le laboratoire juste
avant l'échantillonnage (pas plus de 24 h avant l'échantillonnage), à condition que les éléments en PUF soient
maintenus au frais pour limiter les pertes le plus possible avant l'échantillonnage. Ce mode opératoire peut
éviter la contamination sur site et un problème de sécurité pouvant interdire l'application sur le site.
Surveiller le débit d'air à travers le dispositif d'échantillonnage à l'aide d'un ou de plusieurs régulateurs de
débit. Effectuer un étalonnage multipoint du régulateur de débit tous les six mois à l'aide d'un orifice
d'étalonnage d'audit normalisé, fixé de manière temporaire à l'entrée de l'échantillonneur. En variante, un
compteur à gaz type sec à grand débit peut être utilisé s'il a été validé comme étalon de transfert.
L'échantillonneur doit être étalonné:
a) lorsqu'il est neuf;
b) après des réparations ou des opérations de maintenance majeures;
c) chaque fois qu'un point soumis à un audit s'écarte de la courbe d'étalonnage de plus de 7 %; ou
d) aux intervalles spécifiés dans le manuel d'utilisation.
L'étalonnage et le réétalonnage du compteur à gaz sur le site sont réalisés conformément aux normes de
qualité du laboratoire, par exemple à l'aide d'un étalon de transfert de débit à orifice étalonné.
Dans des conditions peu probables de concentration importante en poussières en suspension dans l'air, le
débit d'air à travers le filtre peut diminuer sensiblement au cours de l'échantillonnage, en particulier en
l'absence d'une régulation automatique de débit. Même avec des pompes à débit contrôlé, la charge du filtre
peut devenir si importante que l'appareillage s'éteint automatiquement. Par conséquent, il convient de
remplacer le filtre si le débit d'air varie de plus de 10 % de la valeur initiale. Le filtre neuf doit également être
marqué avec les étalons de prélèvement.
Si une correction du volume d'échantillonnage dans les conditions normales de température et de pression
(1 013,25 hPa, 273,15 K) est souhaitée, utiliser la température moyenne et la pression d'air moyenne
mesurées pendant l'échantillonnage.
Prendre soin d'installer le dispositif d'échantillonnage de manière qu'il ne soit pas exposé aux courants d'air,
etc. Pour garantir un échantillonnage représentatif, veiller à ce que le taux de renouvellement de l'air de la
pièce pendant la durée de l'échantillonnage soit similaire à celui observé lors d'un usage normal de la pièce.
Pour réduire le plus possible d'éventuelles nuisances sonores dues à l'appareillage d'échantillonnage, il est
possible d'installer celui-ci dans une pièce attenante ou à l'extérieur. Dans ce cas, raccorder le module
d'échantillonnage au système de pompage à l'aide d'un tube (par exemple toile en PVC de forme tubulaire) et
d'un raccord de flexible. Noter toutefois que plus le tube est long, plus la chute de pression et la charge
soumises au système de pompage sont grandes. Des systèmes de pompage de plus petite taille peuvent être
rendus silencieux s'ils sont placés dans des conteneurs en polyuréthanne ou en polystyrène tels que des
glacières. Toutefois, il convient de veiller à l'absence de surchauffe du système.
Pour déterminer une valeur moyenne représentative des concentrations de PCB, PCDD et PCDF dans l'air, il
peut être nécessaire de réaliser l'échantillonnage sur des périodes assez longues. Pour des opérations de
mesurage normales, les volumes prélevés ne doivent pas dépasser 360 m (l'équivalent d'une période
3 3
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. Dans des cas particuliers, des volumes prélevés à l'aide
d'échantillonneurs
...
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