SIST ISO 16000-31:2015
Indoor air - Part 31: Measurement of flame retardants and plasticizers based on organophosphorus compounds - Phosphoric acid ester
Indoor air - Part 31: Measurement of flame retardants and plasticizers based on organophosphorus compounds - Phosphoric acid ester
This part of ISO 16000 specifies a test method for the sampling and analysis of the phosphoric acid
esters in indoor air and in test chamber air through gas chromatography/mass spectrometry. Both
principle methods of the low-resolution mass spectrometry and the high-resolution mass spectrometry
are described.
The methods described in this part of ISO 16000 are not suitable for the determination of the phosphoric
acid esters in materials.
NOTE ISO 16000-6 can be applied for the determination of the more volatile compounds covered by this
standard.
Air intérieur - Partie 31: Mesurage des ignifugeants basés sur des composés organophosphorés - Ester d'acide phosphorique
L'ISO 16000-31:2014 sp�cifie une m�thode d'essai pour pr�lever et analyser les esters d'acide phosphorique dans l'air int�rieur et dans l'air de chambres d'essai par chromatographie en phase gazeuse/spectrom�trie de masse. Deux m�thodes principales, � savoir la spectrom�trie de masse � basse r�solution et la spectrom�trie de masse � haute r�solution, sont d�crites.
Les m�thodes d�crites dans l'ISO 16000-31:2014 ne conviennent pas � la d�termination de la concentration en esters d'acide phosphorique dans les mat�riaux.
Notranji zrak – 31. del: Meritve zaviralnikov plamena in plastifikatorji na osnovi organofosfornih spojin - Ester fosforjeve kisline
Ta del standarda ISO 16000 določa preskusno metodo za vzorčenje in analizo estrov fosforjeve
kisline v notranjem zraku in zraku v preskusnih komorah z plinsko kromatografijo/masno spektrometrijo. Opisani
sta obe glavni metodi masne spektrometrije z nizko resolucijo in masne spektrometrije z visoko resolucijo. Metodi, opisani v tem delu standarda ISO 16000, nista primerni za določanje estrov fosforjeve kisline v materialih.
OPOMBA Standard ISO 16000-6 se lahko uporablja za določanje bolj hlapnih spojin, ki so zajete v tem standardu.
General Information
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Standards Content (Sample)
INTERNATIONAL ISO
STANDARD 16000-31
First edition
2014-05-01
Indoor air —
Part 31:
Measurement of flame retardants
and plasticizers based on
organophosphorus compounds —
Phosphoric acid ester
Air intérieur —
Partie 31: Mesurage des ignifugeants basés sur des composés
organophosphorés — Ester d’acide phosphorique
Reference number
ISO 16000-31:2014(E)
©
ISO 2014
---------------------- Page: 1 ----------------------
ISO 16000-31:2014(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2014
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of
the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2014 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 16000-31:2014(E)
Contents Page
Foreword .iv
Introduction .vi
1 Scope . 1
2 Normative references . 1
3 Occurrence . 1
4 Indoor air . 3
4.1 Measurement planning . 3
4.2 Apparatus and materials for sampling and sample preparation . 3
4.3 Sampling . 6
4.4 Sample preparation . 6
5 Test chamber air . 6
5.1 General . 6
5.2 Apparatus and materials for sampling . 7
5.3 Sampling . 7
5.4 Sampling procedure . 8
5.5 Sample preparation . 8
6 Calibration . 8
6.1 Internal standard solutions and calibration solutions . 8
6.2 Internal standard solutions. 8
6.3 Calibration solutions for low resolution . 9
6.4 Calibration solutions for high resolution .10
7 Identification and quantification .11
7.1 General .11
7.2 Analysis apparatus .11
7.3 Analysis with GC/LR-MS .11
7.4 Analysis with GC/HR-MS .11
7.5 Calculation result interpretation and presentation .13
8 Performance characteristics .14
8.1 Performance characteristics of the air analyses .14
9 Quality assurance .14
10 Interferences .14
Annex A (informative) Nomenclature and physical characteristics .16
Annex B (informative) Example chromatograms for standard solutions .19
Bibliography .21
© ISO 2014 – All rights reserved iii
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ISO 16000-31:2014(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the meaning of ISO specific terms and expressions related to conformity
assessment, as well as information about ISO’s adherence to the WTO principles in the Technical Barriers
to Trade (TBT) see the following URL: Foreword - Supplementary information
The committee responsible for this document is 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 in indoor air and test chamber
air — 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 or 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)
iv © ISO 2014 – All rights reserved
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ISO 16000-31:2014(E)
— 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
— 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 )
2
— Part 16: Detection and enumeration of moulds — Sampling by filtration
— Part 17: Detection and enumeration of moulds — Culture-based method
— Part 18: Detection and enumeration of moulds — Sampling by impaction
— Part 19: Sampling strategy for moulds
— Part 21: Detection and enumeration of moulds — Sampling from materials
— 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 compound (except
formaldehyde) concentrations by sorptive building materials
— Part 25: Determination of the emission of semi-volatile organic compounds by building products —
Micro-chamber method
— Part 26: Sampling strategy for carbon dioxide (CO )
2
— Part 28: Determination of odour emissions from building products using test chambers
— Part 29: Test methods for VOC detectors
— Part 30: Sensory testing of indoor air
— Part 31: Measurement of flame retardants and plasticizers based on organophosphorus compounds —
Phosphoric acid ester
— Part 32: Investigation of buildings for pollutants and other injurious factors — Inspections
The following parts are under preparation:
— Part 33: Determination of phthalates with gas chromatography/mass spectrometry (GC/MS)
— Part 34: Strategies for the measurement of airborne particles (PM 2,5 fraction)
— Part 35: Measurement of polybrominated diphenylether, hexabromocyclododecane and
hexabromobenzene
— Part 36: Test method for the reduction rate of airborne bacteria by air purifiers using a test chamber
© ISO 2014 – All rights reserved v
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ISO 16000-31:2014(E)
Introduction
In general terms, phosphoric acid esters are formed by the reaction of alcohols or phenols with
phosphoryl chloride (POCl ). A distinction is made between mono-, di-, and triesters (see Figure 1). The
3
triesters with aryl and alkyl groups, as well as with mixed halogenated and halogen-free ester groups
serve as plasticizers and flame retardants in plastics and varnishes. Parallel therewith, phosphoric acid
esters are incorporated in hardeners and accelerants, in mordant and adhesion boosting agents, and
serve as cleaning, corrosion inhibition, and adhesion-facilitating substances by the treatment of metal
surfaces. They are used as auxiliary means in paper and textiles, as wetting and defoaming agents,
emulsifiers, and stabilizers, as additives to cleaning agents and detergents, as not readily flammable
hydraulic liquids, and as oil and fuel additives (see Table 1). Not considered in this regard are the groups
of the thio- and dithiophosphoric acid esters (pesticides), as well as the phosphoric acid esters with
[3]
cyanide and halogen groups, with a special impact as acetylcholinesterase inhibitors (nerve gases).
Key
R aryl, alkyl, halogenated, and halogen-free ester groups
Figure 1 — Structural formula of the phosphoric acid esters
Such multiplex applicability of the organophosporus compounds (OPCs) leads to the effect that large
indoor areas with OPC-containing building materials, varnishes, paints, floor care products, or fire
protection coatings can be encountered. Due to their varying physical and physical-chemical properties,
OPC can also be detected in the indoor transfer media (dust and air). As a rule, OPCs boiling at high
temperatures such as tris(2-butoxyethyl) phosphate (TBEP, see Annex A) can be found in relevant
concentrations in indoor air only if the emission source reaches elevated temperatures. In the case of
such sources (e.g. screens or roller blinds for sun protection), the importance of higher temperatures
must be taken into consideration when emission chamber tests are carried out.
There is an increasing public interest in the possible health effects of OPCs indoors. For indoor air, a
3
Guideline Value II of 0,05 mg/m was published for TCEP and, in simplified terms, for the sum of TCEP,
3 [4]
TCPP, TBP, TBEP, TEHP, and TPP as well. The Guideline Value I derived there amounts to 0,005 mg/m .
[5]
A review article on the occurrence and evaluation of OPC in an indoor environment is available.
This part of ISO 16000 is based on VDI 4301 Part 5.
vi © ISO 2014 – All rights reserved
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INTERNATIONAL STANDARD ISO 16000-31:2014(E)
Indoor air —
Part 31:
Measurement of flame retardants and plasticizers based
on organophosphorus compounds — Phosphoric acid ester
1 Scope
This part of ISO 16000 specifies a test method for the sampling and analysis of the phosphoric acid
esters in indoor air and in test chamber air through gas chromatography/mass spectrometry. Both
principle methods of the low-resolution mass spectrometry and the high-resolution mass spectrometry
are described.
The methods described in this part of ISO 16000 are not suitable for the determination of the phosphoric
acid esters in materials.
NOTE ISO 16000-6 can be applied for the determination of the more volatile compounds covered by this
standard.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
ISO 16000-1, Indoor air — Part 1: General aspects of sampling strategy
ISO 16000-9, Indoor air — Part 9: Determination of the emission of volatile organic compounds from
building products and furnishing — Emission test chamber method
ISO 16000-13, 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
3 Occurrence
The following compounds belonging to the halogen-free organophosphates are frequently detected in
indoor air:
— triphenyl phosphate (TPP);
— tris(2-butoxyethyl) phosphate (TBEP);
— tri-n-butyl phosphate (TBP);
— tris(2-ethylhexyl) phosphate (TEHP);
— cresyl diphenyl phosphate (CDP);
— triethyl phosphate (TEP);
— tricresyl phosphate (TCP).
© ISO 2014 – All rights reserved 1
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ISO 16000-31:2014(E)
The following halogenated phosphoric acid esters are detected predominantly in house dust and indoor
air:
— tris(2-chloroethyl) phosphate (TCEP);
— tris(chloropropyl) phosphate (TCPP);
— tris(1,3-dichloro-2-propyl) phosphate (TDCPP).
Bridged diphosphates based on resorcinol- and bisphenol-A are also increasingly implemented as flame
retardants, e. g.
— tetraphenyl resorcinol diphosphate (RDP) or
— tetraphenyl bisphenol-A diphosphate (BDP).
So far, there is little information about the release of these compounds from primary sources.
Table 1 provides an overview of the organophosphates frequently detected in indoor air. The
nomenclature and the chemical and physical data on the organophosphates are listed in Annex A.
[5] [6]
Table 1 — Organophosphates and their intended use (see References and )
OPC Abbrevia- Organophosphates Intended use as flame retardant and plasticizer
tion
CDP Cresyl diphenyl Flame retardant coatings
phosphate
RDP Tetraphenyl resor- Casing materials, special cables
cinol diphosphate
TBEP Tris(2-butoxyethyl) Floor care products, floor wax, additives in elastomers, solvents
phosphate for
resins, antifoaming agents, additives for plastic, synthetic rub-
ber, and varnishes
TBP Tri-n-butyl phos- Defoaming agents for concrete additives, wall paper, dispersion
phate paints, varnishes, rubber, plastic, and vinyl resins, antifoaming
agents
TCEP Tris(2-chloroethyl) Paints, coatings, soundproofing ceilings, fibre glass wall paper,
phosphate expanding foam, casing materials
TCPP Tris(1-chloro- Sound-absorbing polyurethane foam, expansion foam, soft foam
2-propyl)-phos- (seats, mattresses), rear lining of textile, casing materials
a
phate
TDBPP Tris(2,3-dibromo- Foamed rubber, varnishes, paper, paints, cellulose-, triacetate-,
propyl) phosphate and polyester fabrics, carpets, resins, furniture, car interior
details
TDCPP Tris(1,3-dichloro- PU foam, casing materials, rear lining of textile
2-propyl) phosphate
TEHP Tris(2-ethylhexyl) Stabilizers, fat additives, additives for synthetic rubber
phosphate
TCP Tricresyl phosphate Lubricants, car interiors, additives to floor covering and wall
cladding
TPP Triphenyl phosphate Expanding foam, paints and varnishes, brighteners, casing
materials, photographic films, phenol resins, additives for lubri-
cants, car interior details
a
Technical TCPP does not exist as a pure isomer. Hence it usually leads to up to three GC signals.
2 © ISO 2014 – All rights reserved
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ISO 16000-31:2014(E)
The published concentrations of indoor air measurements are compiled in Table 2. Citing of occasion-
relevant measurement values cannot be excluded.
Table 2 — Published results on OPC in indoor air
Substance Concentration in indoor air
3
µg/m
Range Median Reference
TCEP < 0,005 to 6 0,10 to 0,38 [8][9][10]
TCPP 0,019 to – [10]
0,058
TBP 0,01 to 0,064 – [10]
TBEP 0,001 to 0,03 – [9] and[10]
TEHP < 0,001 to – [10]
0,01
TPP < 0,01 – [9] and[10]
TCP < 0,01 – [9]
4 Indoor air
4.1 Measurement planning
The measurement planning for the determination of the indoor air for phosphoric acid esters is
performed according to the requirements of ISO 16000-1.
4.2 Apparatus and materials for sampling and sample preparation
4.2.1 Sampling apparatus
The sampling system is described in detail in ISO 16000-13.
4.2.1.1 Sampling head, with a sleeve for holding the PU foams (Figures 2a and 2b) (see also ISO 16000-
13).
© ISO 2014 – All rights reserved 3
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ISO 16000-31:2014(E)
a) PU foam sleeve with cover (aluminium) b) Sampling head
Key
1 cover
2 O-ring
3 PU foam sleeve (external diameter: 49,5 mm, length: approx. 120 mm)
4 stainless steel mesh
5 cap
6 O-ring
7 PU foam sleeve
8 cylinder (internal diameter: 49,8 mm)
9 stainless steel mesh to carry the glass fibre filter
10 PTFE-ring/filter disc/PTFE-ring
11 cap with inlet bore (internal diameter of the inlet bore: 27 mm)
12 spacer
13 baffle plate
14 O-ring
Figure 2 — Sampling apparatus consisting of a sampling head with a sleeve for holding PU
foams
3 3
4.2.1.2 Pump, with volumetric flow of 2,7 m /h to 2,8 m /h (45 l/min to 46,7 l/min) under sampling
conditions.
4 © ISO 2014 – All rights reserved
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ISO 16000-31:2014(E)
4.2.1.3 Gas volume meter.
4.2.1.4 Hygrometer.
4.2.1.5 Thermometer.
4.2.1.6 Barometer.
1)
NOTE OPC sampling by means of “low-volume sampling systems” (PU foams, e.g. ORBO 1000 ) with
a sampling rate of 1 l/min to 5 l/min is possible within specified limits only. The sampling efficiency of such
adsorbents for airborne particles is not known (see Reference [11]). This procedure does not correspond to the
particle sampling requirements. Hence, its application comparability with the method described herein has to be
proven.
4.2.2 Sample preparation apparatus
4.2.2.1 Glass apparatus, conventional laboratory equipment.
4.2.2.2 Extractor, Soxhlet.
4.2.2.3 Microlitre syringes, 10 µl, 50 µl, and 100 µl.
4.2.3 Materials for the sampling and sample preparation
4.2.3.1 Dichloromethane and toluene, all listed solvents shall be of sufficient purity for trace analysis.
13 13
4.2.3.2 Internal standards, C-γ-HCH and C-DDE (see 6.1).
4.2.3.3 Glass fibre filter, ∅ 5 cm, blank free.
4.2.3.4 PU foam, ∅ 5 cm, length of 2,5 cm, with low contaminations.
Step-by-step cleaning instructions for a “factory new” PU foam:
1) 24 h extraction with methanol in Soxhlet extractor;
2) 24 h extraction with dichloromethane in Soxhlet extractor;
3) 24 h extraction with toluene in Soxhlet extractor;
4) 24 h extraction with acetone in Soxhlet extractor.
Cleaning instructions for a sampled and extracted PU foam:
1) 24 h extraction with toluene in Soxhlet extractor;
2) 24 h extraction with acetone in Soxhlet extractor.
Dry the PU foam in a desiccator under adjacent vacuum conditions and with a gentle ultrapure nitrogen
flow (from the evaporation of liquid nitrogen) or in a vacuum drying cabinet at 40 °C.
PU foams can shrink during extraction or respectively cleaning. Care shall be taken that these remain
precisely fitting after cleaning.
1) ORBO 1000 is the trade name of a commercially available product. This information is given for the convenience
of users of this document and does not constitute an endorsement by ISO of the product named. Equivalent products
may be used if they can be shown to lead to the same results.
© ISO 2014 – All rights reserved 5
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ISO 16000-31:2014(E)
4.3 Sampling
Enrichment of the substances to be analysed from the indoor air takes place on a glass fibre filter and PU
foam under the application of the sampling head as described in ISO 16000-13. Particle-bound as well as
gaseous OPC are sampled in this way.
The internal standard is applied to the PU foam, whereas a total of 100 µl (for LRMS) or 50 µl (for HRMS)
of the internal standard solution (see 6.1 and 6.2.1) are injected at different locations into the foam (e.g.
with a microlitre syringe).
The internal standard should preferably be applied before sampling. If this proves impossible under
justified occasions, the internal standard can also be spiked prior to the extraction, and a note thereof
shall be entered in the test report.
At the measurement location, the PU foam is inserted in the sampling head. The glass fibre filter is
placed in the filter holder by the aid of a pair of tweezers and fixed. The sampling head is positioned
on the stand in such manner that the sampled air will flow through the sampling head in a vertical
direction from the bottom to the top. The suction orifice is located at 1,2 m to 1,5 m above the floor. The
3 3
sampling duration is normally 1 h. The volumetric flow shall be 2,7 m /h to 2,8 m /h. The sampling
volume taken in 1 h should not exceed 10 % of the air exchange rate. If the latter is unknown, then the
hourly drawn sampling volume shall not exceed 10 % of the room volume. The room temperature, the
relative air humidity, and the air pressure shall be measured and recorded immediately prior to and
after the sampling. Upon the sampling completion, the PU foam and the glass fibre filter are removed
from the sampling head and transferred to suitable transportation containers.
4.4 Sample preparation
All deployed glass apparatus are rinsed with dichloromethane (DCM). If no blank-free glass apparatus
can be obtained despite cleaning it with DCM, these shall then be additionally heated up for 24 h at
150 °C in a drying cabinet.
The PU foams and the filter are extracted jointly in a Soxhlet extractor. A minimum of 50 extraction
cycles shall be achieved thereby.
The obtained extract is reduced to a volume of approximately 1 ml to 5 ml in a rotary evaporator under
®2)
a controlled vacuum or in a Turbovap . A further volume reduction to approximately 0,1 ml to 1 ml is
performed by using a flow of pure nitrogen. The solvent shall not be allowed to evaporate completely
because losses of more volatile OPC are very likely. Losses can be prevented by the addition of toluene
as a keeper.
NOTE Gas chromatography retention times can be altered when toluene is applied as a keeper.
Calibration is performed in accordance with Clause 6, and quantification is according to Clause 7.
5 Test chamber air
5.1 General
Emission measurements with building products and consumer goods under controlled climatic
conditions are undertaken in order to establish substance-specific release rates [specific emission rates
[12][13][14]
(SERs)]. The chamber air measurement takes place in a dust-free atmosphere so as to enable a
simplified sampling procedure without particle separation as hereafter described. Care shall be taken
with regard to the chamber volume, air exchange rate, and sampling volume so that the sampling volume
is smaller than the amount of supplied air. The sample preparation, and in particular the sample storage,
shall be coordinated with the test chamber measurement.
2) Turbovap is the trade name of a commercially available product. This information is given for the convenience of
users of this document and does not constitute an endorsement by ISO of the product named. Equivalent products
may be used if they can be shown to lead to the same results.
6 © ISO 2014 – All rights reserved
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ISO 16000-31:2014(E)
Due to the physical properties of the compound class, the measurement of the OPC emissions from
building products and from devices for indoor use is a complex process. Principally, such emissions can
be determined by the chamber analyses according to ISO 16000-9. If ISO 16000-9 developed for volatile
organic compounds (VOCs) is applied to semi-volatile OPC (SVOC), the specific chamber properties (e.g.
[14][15]
sink effects) shall be taken into consideration. A precondition for performing the test chamber
analyses is the knowledge of ISO 16000-9.
5.2 Apparatus and materials for sampling
5.2.1 Emission test chamber, according to ISO 16000-9.
5.2.2 Sampling pump.
5.2.3 Gas volume meter.
5.2.4 Glass apparatus, conventional laboratory equipment.
5.2.5 Extractor, Soxhlet.
5.2.6 Microlitre syringes, 10 µl, 50 µl, and 100 µl.
13 13
5.2.7 Internal standards, C-γ-HCH or C-DDE (see 6.1).
3)
®
5.2.8 Adsorbents, XAD-2 or PU foam.
5.2.9 Quartz wool, silanized quartz wool.
The pre-cleaning is performed by Soxhlet extraction with methanol for at least 14 h.
5.3 Sampling
5.3.1 Chamber preparation
The chamber is cleaned prior to the start of the emission
...
SLOVENSKI STANDARD
SIST ISO 16000-31:2015
01-april-2015
Notranji zrak – 31. del: Meritve zaviralnikov plamena in plastifikatorji na osnovi
organofosfornih spojin - Ester fosforjeve kisline
Indoor air - Part 31: Measurement of flame retardants and plasticizers based on
organophosphorus compounds - Phosphoric acid ester
Air intérieur - Partie 31: Mesurage des ignifugeants basés sur des composés
organophosphorés - Ester d'acide phosphorique
Ta slovenski standard je istoveten z: ISO 16000-31:2014
ICS:
13.040.20 Kakovost okoljskega zraka Ambient atmospheres
SIST ISO 16000-31:2015 en,fr
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST ISO 16000-31:2015
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SIST ISO 16000-31:2015
INTERNATIONAL ISO
STANDARD 16000-31
First edition
2014-05-01
Indoor air —
Part 31:
Measurement of flame retardants
and plasticizers based on
organophosphorus compounds —
Phosphoric acid ester
Air intérieur —
Partie 31: Mesurage des ignifugeants basés sur des composés
organophosphorés — Ester d’acide phosphorique
Reference number
ISO 16000-31:2014(E)
©
ISO 2014
---------------------- Page: 3 ----------------------
SIST ISO 16000-31:2015
ISO 16000-31:2014(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2014
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of
the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2014 – All rights reserved
---------------------- Page: 4 ----------------------
SIST ISO 16000-31:2015
ISO 16000-31:2014(E)
Contents Page
Foreword .iv
Introduction .vi
1 Scope . 1
2 Normative references . 1
3 Occurrence . 1
4 Indoor air . 3
4.1 Measurement planning . 3
4.2 Apparatus and materials for sampling and sample preparation . 3
4.3 Sampling . 6
4.4 Sample preparation . 6
5 Test chamber air . 6
5.1 General . 6
5.2 Apparatus and materials for sampling . 7
5.3 Sampling . 7
5.4 Sampling procedure . 8
5.5 Sample preparation . 8
6 Calibration . 8
6.1 Internal standard solutions and calibration solutions . 8
6.2 Internal standard solutions. 8
6.3 Calibration solutions for low resolution . 9
6.4 Calibration solutions for high resolution .10
7 Identification and quantification .11
7.1 General .11
7.2 Analysis apparatus .11
7.3 Analysis with GC/LR-MS .11
7.4 Analysis with GC/HR-MS .11
7.5 Calculation result interpretation and presentation .13
8 Performance characteristics .14
8.1 Performance characteristics of the air analyses .14
9 Quality assurance .14
10 Interferences .14
Annex A (informative) Nomenclature and physical characteristics .16
Annex B (informative) Example chromatograms for standard solutions .19
Bibliography .21
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Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the meaning of ISO specific terms and expressions related to conformity
assessment, as well as information about ISO’s adherence to the WTO principles in the Technical Barriers
to Trade (TBT) see the following URL: Foreword - Supplementary information
The committee responsible for this document is 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 in indoor air and test chamber
air — 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 or 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)
iv © ISO 2014 – All rights reserved
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SIST ISO 16000-31:2015
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— 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
— 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 )
2
— Part 16: Detection and enumeration of moulds — Sampling by filtration
— Part 17: Detection and enumeration of moulds — Culture-based method
— Part 18: Detection and enumeration of moulds — Sampling by impaction
— Part 19: Sampling strategy for moulds
— Part 21: Detection and enumeration of moulds — Sampling from materials
— 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 compound (except
formaldehyde) concentrations by sorptive building materials
— Part 25: Determination of the emission of semi-volatile organic compounds by building products —
Micro-chamber method
— Part 26: Sampling strategy for carbon dioxide (CO )
2
— Part 28: Determination of odour emissions from building products using test chambers
— Part 29: Test methods for VOC detectors
— Part 30: Sensory testing of indoor air
— Part 31: Measurement of flame retardants and plasticizers based on organophosphorus compounds —
Phosphoric acid ester
— Part 32: Investigation of buildings for pollutants and other injurious factors — Inspections
The following parts are under preparation:
— Part 33: Determination of phthalates with gas chromatography/mass spectrometry (GC/MS)
— Part 34: Strategies for the measurement of airborne particles (PM 2,5 fraction)
— Part 35: Measurement of polybrominated diphenylether, hexabromocyclododecane and
hexabromobenzene
— Part 36: Test method for the reduction rate of airborne bacteria by air purifiers using a test chamber
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Introduction
In general terms, phosphoric acid esters are formed by the reaction of alcohols or phenols with
phosphoryl chloride (POCl ). A distinction is made between mono-, di-, and triesters (see Figure 1). The
3
triesters with aryl and alkyl groups, as well as with mixed halogenated and halogen-free ester groups
serve as plasticizers and flame retardants in plastics and varnishes. Parallel therewith, phosphoric acid
esters are incorporated in hardeners and accelerants, in mordant and adhesion boosting agents, and
serve as cleaning, corrosion inhibition, and adhesion-facilitating substances by the treatment of metal
surfaces. They are used as auxiliary means in paper and textiles, as wetting and defoaming agents,
emulsifiers, and stabilizers, as additives to cleaning agents and detergents, as not readily flammable
hydraulic liquids, and as oil and fuel additives (see Table 1). Not considered in this regard are the groups
of the thio- and dithiophosphoric acid esters (pesticides), as well as the phosphoric acid esters with
[3]
cyanide and halogen groups, with a special impact as acetylcholinesterase inhibitors (nerve gases).
Key
R aryl, alkyl, halogenated, and halogen-free ester groups
Figure 1 — Structural formula of the phosphoric acid esters
Such multiplex applicability of the organophosporus compounds (OPCs) leads to the effect that large
indoor areas with OPC-containing building materials, varnishes, paints, floor care products, or fire
protection coatings can be encountered. Due to their varying physical and physical-chemical properties,
OPC can also be detected in the indoor transfer media (dust and air). As a rule, OPCs boiling at high
temperatures such as tris(2-butoxyethyl) phosphate (TBEP, see Annex A) can be found in relevant
concentrations in indoor air only if the emission source reaches elevated temperatures. In the case of
such sources (e.g. screens or roller blinds for sun protection), the importance of higher temperatures
must be taken into consideration when emission chamber tests are carried out.
There is an increasing public interest in the possible health effects of OPCs indoors. For indoor air, a
3
Guideline Value II of 0,05 mg/m was published for TCEP and, in simplified terms, for the sum of TCEP,
3 [4]
TCPP, TBP, TBEP, TEHP, and TPP as well. The Guideline Value I derived there amounts to 0,005 mg/m .
[5]
A review article on the occurrence and evaluation of OPC in an indoor environment is available.
This part of ISO 16000 is based on VDI 4301 Part 5.
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INTERNATIONAL STANDARD ISO 16000-31:2014(E)
Indoor air —
Part 31:
Measurement of flame retardants and plasticizers based
on organophosphorus compounds — Phosphoric acid ester
1 Scope
This part of ISO 16000 specifies a test method for the sampling and analysis of the phosphoric acid
esters in indoor air and in test chamber air through gas chromatography/mass spectrometry. Both
principle methods of the low-resolution mass spectrometry and the high-resolution mass spectrometry
are described.
The methods described in this part of ISO 16000 are not suitable for the determination of the phosphoric
acid esters in materials.
NOTE ISO 16000-6 can be applied for the determination of the more volatile compounds covered by this
standard.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
ISO 16000-1, Indoor air — Part 1: General aspects of sampling strategy
ISO 16000-9, Indoor air — Part 9: Determination of the emission of volatile organic compounds from
building products and furnishing — Emission test chamber method
ISO 16000-13, 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
3 Occurrence
The following compounds belonging to the halogen-free organophosphates are frequently detected in
indoor air:
— triphenyl phosphate (TPP);
— tris(2-butoxyethyl) phosphate (TBEP);
— tri-n-butyl phosphate (TBP);
— tris(2-ethylhexyl) phosphate (TEHP);
— cresyl diphenyl phosphate (CDP);
— triethyl phosphate (TEP);
— tricresyl phosphate (TCP).
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The following halogenated phosphoric acid esters are detected predominantly in house dust and indoor
air:
— tris(2-chloroethyl) phosphate (TCEP);
— tris(chloropropyl) phosphate (TCPP);
— tris(1,3-dichloro-2-propyl) phosphate (TDCPP).
Bridged diphosphates based on resorcinol- and bisphenol-A are also increasingly implemented as flame
retardants, e. g.
— tetraphenyl resorcinol diphosphate (RDP) or
— tetraphenyl bisphenol-A diphosphate (BDP).
So far, there is little information about the release of these compounds from primary sources.
Table 1 provides an overview of the organophosphates frequently detected in indoor air. The
nomenclature and the chemical and physical data on the organophosphates are listed in Annex A.
[5] [6]
Table 1 — Organophosphates and their intended use (see References and )
OPC Abbrevia- Organophosphates Intended use as flame retardant and plasticizer
tion
CDP Cresyl diphenyl Flame retardant coatings
phosphate
RDP Tetraphenyl resor- Casing materials, special cables
cinol diphosphate
TBEP Tris(2-butoxyethyl) Floor care products, floor wax, additives in elastomers, solvents
phosphate for
resins, antifoaming agents, additives for plastic, synthetic rub-
ber, and varnishes
TBP Tri-n-butyl phos- Defoaming agents for concrete additives, wall paper, dispersion
phate paints, varnishes, rubber, plastic, and vinyl resins, antifoaming
agents
TCEP Tris(2-chloroethyl) Paints, coatings, soundproofing ceilings, fibre glass wall paper,
phosphate expanding foam, casing materials
TCPP Tris(1-chloro- Sound-absorbing polyurethane foam, expansion foam, soft foam
2-propyl)-phos- (seats, mattresses), rear lining of textile, casing materials
a
phate
TDBPP Tris(2,3-dibromo- Foamed rubber, varnishes, paper, paints, cellulose-, triacetate-,
propyl) phosphate and polyester fabrics, carpets, resins, furniture, car interior
details
TDCPP Tris(1,3-dichloro- PU foam, casing materials, rear lining of textile
2-propyl) phosphate
TEHP Tris(2-ethylhexyl) Stabilizers, fat additives, additives for synthetic rubber
phosphate
TCP Tricresyl phosphate Lubricants, car interiors, additives to floor covering and wall
cladding
TPP Triphenyl phosphate Expanding foam, paints and varnishes, brighteners, casing
materials, photographic films, phenol resins, additives for lubri-
cants, car interior details
a
Technical TCPP does not exist as a pure isomer. Hence it usually leads to up to three GC signals.
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The published concentrations of indoor air measurements are compiled in Table 2. Citing of occasion-
relevant measurement values cannot be excluded.
Table 2 — Published results on OPC in indoor air
Substance Concentration in indoor air
3
µg/m
Range Median Reference
TCEP < 0,005 to 6 0,10 to 0,38 [8][9][10]
TCPP 0,019 to – [10]
0,058
TBP 0,01 to 0,064 – [10]
TBEP 0,001 to 0,03 – [9] and[10]
TEHP < 0,001 to – [10]
0,01
TPP < 0,01 – [9] and[10]
TCP < 0,01 – [9]
4 Indoor air
4.1 Measurement planning
The measurement planning for the determination of the indoor air for phosphoric acid esters is
performed according to the requirements of ISO 16000-1.
4.2 Apparatus and materials for sampling and sample preparation
4.2.1 Sampling apparatus
The sampling system is described in detail in ISO 16000-13.
4.2.1.1 Sampling head, with a sleeve for holding the PU foams (Figures 2a and 2b) (see also ISO 16000-
13).
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a) PU foam sleeve with cover (aluminium) b) Sampling head
Key
1 cover
2 O-ring
3 PU foam sleeve (external diameter: 49,5 mm, length: approx. 120 mm)
4 stainless steel mesh
5 cap
6 O-ring
7 PU foam sleeve
8 cylinder (internal diameter: 49,8 mm)
9 stainless steel mesh to carry the glass fibre filter
10 PTFE-ring/filter disc/PTFE-ring
11 cap with inlet bore (internal diameter of the inlet bore: 27 mm)
12 spacer
13 baffle plate
14 O-ring
Figure 2 — Sampling apparatus consisting of a sampling head with a sleeve for holding PU
foams
3 3
4.2.1.2 Pump, with volumetric flow of 2,7 m /h to 2,8 m /h (45 l/min to 46,7 l/min) under sampling
conditions.
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4.2.1.3 Gas volume meter.
4.2.1.4 Hygrometer.
4.2.1.5 Thermometer.
4.2.1.6 Barometer.
1)
NOTE OPC sampling by means of “low-volume sampling systems” (PU foams, e.g. ORBO 1000 ) with
a sampling rate of 1 l/min to 5 l/min is possible within specified limits only. The sampling efficiency of such
adsorbents for airborne particles is not known (see Reference [11]). This procedure does not correspond to the
particle sampling requirements. Hence, its application comparability with the method described herein has to be
proven.
4.2.2 Sample preparation apparatus
4.2.2.1 Glass apparatus, conventional laboratory equipment.
4.2.2.2 Extractor, Soxhlet.
4.2.2.3 Microlitre syringes, 10 µl, 50 µl, and 100 µl.
4.2.3 Materials for the sampling and sample preparation
4.2.3.1 Dichloromethane and toluene, all listed solvents shall be of sufficient purity for trace analysis.
13 13
4.2.3.2 Internal standards, C-γ-HCH and C-DDE (see 6.1).
4.2.3.3 Glass fibre filter, ∅ 5 cm, blank free.
4.2.3.4 PU foam, ∅ 5 cm, length of 2,5 cm, with low contaminations.
Step-by-step cleaning instructions for a “factory new” PU foam:
1) 24 h extraction with methanol in Soxhlet extractor;
2) 24 h extraction with dichloromethane in Soxhlet extractor;
3) 24 h extraction with toluene in Soxhlet extractor;
4) 24 h extraction with acetone in Soxhlet extractor.
Cleaning instructions for a sampled and extracted PU foam:
1) 24 h extraction with toluene in Soxhlet extractor;
2) 24 h extraction with acetone in Soxhlet extractor.
Dry the PU foam in a desiccator under adjacent vacuum conditions and with a gentle ultrapure nitrogen
flow (from the evaporation of liquid nitrogen) or in a vacuum drying cabinet at 40 °C.
PU foams can shrink during extraction or respectively cleaning. Care shall be taken that these remain
precisely fitting after cleaning.
1) ORBO 1000 is the trade name of a commercially available product. This information is given for the convenience
of users of this document and does not constitute an endorsement by ISO of the product named. Equivalent products
may be used if they can be shown to lead to the same results.
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4.3 Sampling
Enrichment of the substances to be analysed from the indoor air takes place on a glass fibre filter and PU
foam under the application of the sampling head as described in ISO 16000-13. Particle-bound as well as
gaseous OPC are sampled in this way.
The internal standard is applied to the PU foam, whereas a total of 100 µl (for LRMS) or 50 µl (for HRMS)
of the internal standard solution (see 6.1 and 6.2.1) are injected at different locations into the foam (e.g.
with a microlitre syringe).
The internal standard should preferably be applied before sampling. If this proves impossible under
justified occasions, the internal standard can also be spiked prior to the extraction, and a note thereof
shall be entered in the test report.
At the measurement location, the PU foam is inserted in the sampling head. The glass fibre filter is
placed in the filter holder by the aid of a pair of tweezers and fixed. The sampling head is positioned
on the stand in such manner that the sampled air will flow through the sampling head in a vertical
direction from the bottom to the top. The suction orifice is located at 1,2 m to 1,5 m above the floor. The
3 3
sampling duration is normally 1 h. The volumetric flow shall be 2,7 m /h to 2,8 m /h. The sampling
volume taken in 1 h should not exceed 10 % of the air exchange rate. If the latter is unknown, then the
hourly drawn sampling volume shall not exceed 10 % of the room volume. The room temperature, the
relative air humidity, and the air pressure shall be measured and recorded immediately prior to and
after the sampling. Upon the sampling completion, the PU foam and the glass fibre filter are removed
from the sampling head and transferred to suitable transportation containers.
4.4 Sample preparation
All deployed glass apparatus are rinsed with dichloromethane (DCM). If no blank-free glass apparatus
can be obtained despite cleaning it with DCM, these shall then be additionally heated up for 24 h at
150 °C in a drying cabinet.
The PU foams and the filter are extracted jointly in a Soxhlet extractor. A minimum of 50 extraction
cycles shall be achieved thereby.
The obtained extract is reduced to a volume of approximately 1 ml to 5 ml in a rotary evaporator under
®2)
a controlled vacuum or in a Turbovap . A further volume reduction to approximately 0,1 ml to 1 ml is
performed by using a flow of pure nitrogen. The solvent shall not be allowed to evaporate completely
because losses of more volatile OPC are very likely. Losses can be prevented by the addition of toluene
as a keeper.
NOTE Gas chromatography retention times can be altered when toluene is applied as a keeper.
Calibration is performed in accordance with Clause 6, and quantification is according to Clause 7.
5 Test chamber air
5.1 General
Emission measurements with building products and consumer goods under controlled climatic
conditions are undertaken in order to establish substance-specific release rates [specific emission rates
[12][13][14]
(SERs)]. The chamber air measurement takes place in a dust-free atmosphere so as to enable a
simplified sampling procedure without particle separation as hereafter described. Care shall be taken
with regard to the chamber volume, air exchange rate, and sampling volume so that the sampling volume
is smaller than the amount of supplied air. The sample preparation, and in particular the sample storage,
shall be coordinated with the test chamber measurement.
2) Turbovap is the trade name of a commercially available product. This information is given for the convenience of
users of this document and does not constitute an endorsement by ISO of the product named. Equivalent products
may be used if they can be shown to lead to the same results.
6 © ISO 2014 – All rights reserved
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ISO 16000-31:201
...
NORME ISO
INTERNATIONALE 16000-31
Première édition
2014-05-01
Air intérieur —
Partie 31:
Mesurage des ignifugeants basés sur
des composés organophosphorés —
Ester d’acide phosphorique
Indoor air —
Part 31: Measurement of flame retardants and plasticizers based on
organophosphorus compounds — Phosphoric acid ester
Numéro de référence
ISO 16000-31:2014(F)
©
ISO 2014
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ISO 16000-31:2014(F)
DOCUMENT PROTÉGÉ PAR COPYRIGHT
© ISO 2014
Droits de reproduction réservés. Sauf indication contraire, aucune partie de cette publication ne peut être reproduite ni utilisée
sous quelque forme que ce soit et par aucun procédé, électronique ou mécanique, y compris la photocopie, l’affichage sur
l’internet ou sur un Intranet, sans autorisation écrite préalable. Les demandes d’autorisation peuvent être adressées à l’ISO à
l’adresse ci-après ou au comité membre de l’ISO dans le pays du demandeur.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Publié en Suisse
ii © ISO 2014 – Tous droits réservés
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ISO 16000-31:2014(F)
Sommaire Page
Avant-propos .iv
Introduction .vii
1 Domaine d’application . 1
2 Références normatives . 1
3 Occurrence . 1
4 Air intérieur . 3
4.1 Planification du mesurage . 3
4.2 Appareillage et matériaux d’échantillonnage et de préparation des échantillons . 3
4.3 Échantillonnage . 6
4.4 Préparation des échantillons . 6
5 Air de la chambre d’essai . 7
5.1 Généralités . 7
5.2 Appareillage et matériaux d’échantillonnage. 7
5.3 Échantillonnage . 7
5.4 Mode opératoire d’échantillonnage . 8
5.5 Préparation des échantillons . 8
6 Étalonnage . 8
6.1 Solutions d’étalons internes et solutions d’étalonnage . 8
6.2 Solutions d’étalons internes . 9
6.3 Solutions d’étalonnage pour basse résolution. 9
6.4 Solutions d’étalonnage pour haute résolution .10
7 Identification et quantification .11
7.1 Généralités .11
7.2 Matériel d’analyse .11
7.3 Analyse par CPG-SMBR .11
7.4 Analyse par CPG-SMHR .12
7.5 Interprétation et présentation du résultat du calcul.14
8 Caractéristiques de performance .14
8.1 Caractéristiques de performance des analyses d’air .14
9 Assurance qualité .15
10 Interférences .15
Annexe A (informative) Nomenclature et caractéristiques physiques .16
Annexe B (informative) Exemple de chromatogrammes pour des solutions étalons .18
Bibliographie .20
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ISO 16000-31:2014(F)
Avant-propos
L’ISO (Organisation internationale de normalisation) est une fédération mondiale d’organismes
nationaux de normalisation (comités membres de l’ISO). L’élaboration des Normes internationales est
en général confiée aux comités techniques de l’ISO. Chaque comité membre intéressé par une étude
a le droit de faire partie du comité technique créé à cet effet. Les organisations internationales,
gouvernementales et non gouvernementales, en liaison avec l’ISO participent également aux travaux.
L’ISO collabore étroitement avec la Commission électrotechnique internationale (IEC) en ce qui concerne
la normalisation électrotechnique.
Les procédures utilisées pour élaborer le présent document et celles destinées à sa mise à jour sont
décrites dans les Directives ISO/IEC, Partie 1. Il convient, en particulier de prendre note des différents
critères d’approbation requis pour les différents types de documents ISO. Le présent document a été
rédigé conformément aux règles de rédaction données dans les Directives ISO/IEC, Partie 2 (voir www.
iso.org/directives).
L’attention est appelée sur le fait que certains des éléments du présent document peuvent faire l’objet de
droits de propriété intellectuelle ou de droits analogues. L’ISO ne saurait être tenue pour responsable
de ne pas avoir identifié de tels droits de propriété et averti de leur existence. Les détails concernant les
références aux droits de propriété intellectuelle ou autres droits analogues identifiés lors de l’élaboration
du document sont indiqués dans l’Introduction et/ou dans la liste des déclarations de brevets reçues par
l’ISO (voir www.iso.org/brevets).
Les appellations commerciales éventuellement mentionnées dans le présent document sont données
pour information, par souci de commodité, à l’intention des utilisateurs et ne sauraient constituer un
engagement.
Pour une explication de la signification des termes et expressions spécifiques de l’ISO liés à l’évaluation de
la conformité, ou pour toute information au sujet de l’adhésion de l’ISO aux principes de l’OMC concernant
les obstacles techniques au commerce (OTC), voir le lien suivant: Avant-propos — Informations
supplémentaires.
Le comité chargé de l’élaboration du présent document est l’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 dans l’air intérieur et dans l’air des
chambres d’essai — 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
iv © ISO 2014 – Tous droits réservés
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ISO 16000-31:2014(F)
— 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)
— 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)/polychloro-dibenzofuranes (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)
2
— Partie 16: Détection et dénombrement des moisissures — Échantillonnage par filtration
— Partie 17: Détection et dénombrement des moisissures — Méthode par culture
— Partie 18: Détection et dénombrement des moisissures — Échantillonnage par impaction
— Partie 19: Stratégie d’échantillonnage des moisissures
— Partie 21: Détection et dénombrement des moisissures — Échantillonnage à partir de matériaux
— 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 carbonylés sans formaldéhyde, par des matériaux de construction
sorptifs
— Partie 25: Dosage de l’émission de composés organiques semi-volatils de produits de construction —
Méthode de la micro-chambre
— Partie 26: Stratégie de mesure du dioxyde de carbone (CO)
2
— Partie 28: Détermination des émissions d’odeurs des produits de construction au moyen de chambres
d’essai
— Partie 30: Essai sensoriel de l’air intérieur
— Partie 29: Méthodes d’essai pour détecteurs de composés organiques volatils (COV)
— Partie 31: Mesurage des ignifugeants basés sur des composés organophosphorés — Ester d’acide
phosphorique
— Partie 32: Investigation de polluants et autres facteurs nocifs dans les constructions — Inspections
Les parties suivantes sont en cours de préparation:
— Partie 33: Dosage des phtalates par chromatographie en phase gazeuse/spectrométrie de masse
(CPG/SM)
— Partie 34: Stratégies pour le mesurage des particules en suspension (fraction PM 2,5)
— Partie 35: Mesurage des diphényléther polybromé, hexabromocyclododécane et hexabromobenzène
© ISO 2014 – Tous droits réservés v
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ISO 16000-31:2014(F)
— Partie 36: Méthode d’essai pour le taux de réduction des bactéries en suspension par des purificateurs
d’air en utilisant une chambre d’essai
vi © ISO 2014 – Tous droits réservés
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ISO 16000-31:2014(F)
Introduction
En général, les esters d’acide phosphorique sont formés par réaction d’alcools ou de phénols avec du
chlorure de phosphoryle (POCl ). Une distinction entre les mono-, les di- et les triesters est faite (voir
3
la Figure 1). Les triesters contenant des groupes aryle et alkyle ainsi que des groupes mixtes d’esters
halogénés et non halogénés sont utilisés comme plastifiants et ignifugeants dans les matières plastiques
et les vernis. En parallèle, les esters d’acide phosphorique sont incorporés dans les durcissants et les
accélérateurs, dans les agents favorisant le mordant et l’adhérence et sont utilisés comme substances
facilitant le nettoyage, l’adhérence et l’inhibition de la corrosion par le traitement des surfaces
métalliques. Ils sont utilisés en tant que substances auxiliaires dans le papier et les textiles, agents
antimousse, émulsifiants, stabilisants, additifs dans les agents nettoyants et détergents, liquides
hydrauliques difficilement inflammables et additifs pétroliers (voir le Tableau 1). Ne sont pas pris en
compte à cet égard les groupes des esters d’acide thio- et dithiophosphorique (pesticides) ainsi que les
esters d’acide phosphorique contenant du cyanure et des groupes halogénés qui ont un impact spécial
[3]
en tant qu’inhibiteurs de l’acétylcholinestérase (gaz neurotoxiques).
Légende
R groupe aryle, groupe alkyle et groupes d’esters halogénés et non halogénés
Figure 1 — Formule structurale des esters d’acide phosphorique
Cette applicabilité multiplexe des composés organophosphorés (COP) a pour conséquence la création
de grands espaces intérieurs utilisant des matériaux de construction, des vernis, des peintures, des
produits de nettoyage du sol ou des revêtements ignifuges contenant des COP. En raison de leurs
propriétés physiques et physicochimiques variables, les COP peuvent être également détectés dans
les milieux de transfert intérieurs (poussière et air). En règle générale, les COP ayant une température
d’ébullition élevée, par exemple le tris(2-butoxyéthyl) phosphate (TBEP, voir l’Annexe A) peuvent être
retrouvés en concentrations importantes dans l’air intérieur, seulement si la source d’émission a atteint
des températures élevées. Dans le cas de ce type de sources (par exemple, filtres ou stores pare-soleil),
l’influence de hautes températures doit être prise en compte lors de la réalisation d’essais en chambre
d’émission.
Le public porte un intérêt croissant aux éventuels effets sur la santé des COP présents dans l’air intérieur.
3
Pour l’air intérieur, une valeur guide II de 0,05 mg/m a été publiée pour le TCEP et, pour simplifier, pour
l’ensemble des TCEP, TCPP, TBP, TBEP, TEHP et TPP également. La valeur guide I qui en découle s’élève
3 [4]
à 0,005 mg/m . Un article scientifique sur l’occurrence et l’évaluation des COP dans l’air intérieur est
[5]
disponible.
La présente partie de l’ISO 16000 repose sur la VDI 4301 Part 5.
© ISO 2014 – Tous droits réservés vii
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NORME INTERNATIONALE ISO 16000-31:2014(F)
Air intérieur —
Partie 31:
Mesurage des ignifugeants basés sur des composés
organophosphorés — Ester d’acide phosphorique
1 Domaine d’application
La présente partie de l’ISO 16000 spécifie une méthode d’essai pour prélever et analyser les esters
d’acide phosphorique dans l’air intérieur et dans l’air de chambres d’essai par chromatographie en
phase gazeuse/spectrométrie de masse. Deux méthodes principales, à savoir la spectrométrie de masse
à basse résolution et la spectrométrie de masse à haute résolution, sont décrites.
Les méthodes décrites dans la présente partie de l’ISO 16000 ne conviennent pas à la détermination de
la concentration en esters d’acide phosphorique dans les matériaux.
NOTE L’ISO 16000 6 peut être appliqué pour la détermination des composés les plus volatils couverts par
cette norme.
2 Références normatives
Les documents ci-après, dans leur intégralité ou non, sont des références normatives indispensables à
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 16000-1, Air intérieur — Partie 1: Aspects généraux de la stratégie d’échantillonnage
ISO 16000-9, Air intérieur — 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
ISO 16000-13, 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
3 Occurrence
Les composés suivants, du groupe des organophosphates non halogénés, sont fréquemment détectés
dans l’air intérieur:
— le triphénylphosphate (TPP);
— le tris(2-butoxyéthyl) phosphate (TBEP);
— le tri-n-butylphosphate (TBP);
— le tris(2-éthylhexyl) phosphate (TEHP);
— le crésyldiphénylphosphate (CDP);
— le triéthylphosphate (TEP);
— le tricrésylphosphate (TCP).
© ISO 2014 – Tous droits réservés 1
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ISO 16000-31:2014(F)
Les esters halogénés d’acide phosphorique suivants sont principalement détectés dans la poussière des
maisons et dans l’air intérieur:
— le tris(2-chloroéthyl) phosphate (TCEP);
— le tris(chloropropyl) phosphate (TCPP);
— le tris(1,3-dichloro-2-propyl) phosphate (TDCPP).
Les disphosphates pontés à base de résorcinol et de bisphénol A sont également de plus en plus utilisés
comme ignifugeants, par exemple:
— le résorcinoldiphosphate (RDP) de tétraphényle ou
— le bisphénol A-diphosphate (BDP) de tétraphényle.
Pour l’heure, il n’existe que peu d’informations sur le relargage de ces composés émanant de sources
primaires.
Le Tableau 1 donne une vue d’ensemble des organosphosphates fréquemment détectés dans l’air intérieur.
L’Annexe A répertorie la nomenclature et les données physicochimiques des organophosphates.
[5] [6]
Tableau 1 — Organophosphates et leur utilisation prévue (voir les Références et )
Abréviation du Organophosphates Utilisation prévue en tant qu’ignifugeant et plastifiant
COP
CDP Crésyldiphénylphos- Revêtements ignifuges
phate
RDP Résorcinoldiphosphate Matériaux de conditionnement, câbles spéciaux
de tétraphényle
TBEP Tris(2-butoxyéthyl) Produits de nettoyage du sol, encaustique, additifs pour élastomères,
phosphate solvants pour résines, agents antimousse, additifs pour matières plas-
tiques, caoutchouc synthétique et vernis
TBP Tri-n-butylphosphate Agents antimousse pour additifs pour béton, papiers peints, pein-
tures-dispersions, vernis, caoutchouc, résines plastiques et viny-
liques, agents antimousse
TCEP Tris(2-chloréthyl) Peintures, revêtements, plafonds insonorisés, papier peint en fibres
phosphate de verre, mousse expansée, matériaux de conditionnement
TCPP Tris(1-chloro-2-pro- Mousse de polyuréthane à propriétés insonorisantes, mousse expan-
pyl) phosphate sée, mousse souple (sièges, matelas), doublure textile, matériaux de
conditionnement
TDBPP Tris(2,3-dibromopro- Caoutchouc mousse, vernis, papier, peintures, tissus en cellulose,
pyl) phosphate triacétate et polyester, tapis, résines, mobilier, habillages intérieurs
d’automobiles
TDCPP Tris(1,3-dichloro- Mousse de polyuréthane, matériaux de conditionnement, doublure
2-propyl) phosphate textile
TEHP Tris(2-éthylhexyl) Stabilisants, additifs gras, additifs pour caoutchouc synthétique
phosphate
TCP Tricrésylphosphate Lubrifiants, habillages intérieurs d’automobiles, additifs pour revête-
ments de sol et muraux
TPP Triphénylphosphate Mousse expansée, peintures et vernis, azurants optiques, matériaux
de conditionnement, pellicules photographiques, résines phénoliques,
additifs pour lubrifiants, habillages intérieurs d’automobiles
a
Le TCPP technique n’existe pas sous la forme d’un isomère pur. Par conséquent, il provoque généralement l’émission de
trois signaux CPG.
Les concentrations publiées des mesurages dans l’air intérieur sont répertoriées dans le Tableau 2. Il ne
peut être exclu de mentionner des valeurs de mesure propres à un événement.
2 © ISO 2014 – Tous droits réservés
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ISO 16000-31:2014(F)
Tableau 2 — Résultats publiés pour les COP dans l’air intérieur
Substance Concentration dans l’air intérieur
3
µg/m
Gamme Moyenne Référence
TCEP < 0,005 à 6 0,10 à 0,38 [8][9][10]
TCPP 0,019 à 0,058 – [10]
TBP 0,01 à 0,064 – [10]
TBEP 0,001 à 0,03 – [9] et [10]
TEHP < 0,001 à 0,01 – [10]
TPP < 0,01 – [9] et [10]
TCP < 0,01 – [9]
4 Air intérieur
4.1 Planification du mesurage
La planification du mesurage pour déterminer la concentration en esters d’acide phosphorique dans l’air
intérieur est effectuée conformément aux exigences de l’ISO 16000-1.
4.2 Appareillage et matériaux d’échantillonnage et de préparation des échantillons
4.2.1 Appareil d’échantillonnage
Le dispositif d’échantillonnage est décrit en détail dans l’ISO 16000-13.
4.2.1.1 Tête de prélèvement, équipée d’un manchon pour retenir les mousses de polyuréthane
(Figures 2a et 2b) (voir également l’ISO 16000-13).
© ISO 2014 – Tous droits réservés 3
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ISO 16000-31:2014(F)
a) Manchon en mousse de polyuréthane avec b) Tête de prélèvement
couvercle (aluminium)
Légende
1 couvercle
2 joint torique
3 manchon en mousse de polyuréthane (diamètre extérieur: 49,5 mm, longueur: environ 120 mm)
4 tamis en acier inoxydable
5 couvercle
6 joint torique
7 manchon en mousse de polyuréthane
8 cylindre (diamètre intérieur: 49,8 mm)
9 tamis en acier inoxydable pour supporter le filtre en fibre de verre
10 bague en PTFE/disque de filtration/bague en PTFE
11 couvercle avec orifice d’entrée (diamètre intérieur de l’orifice d’entrée: 27 mm)
12 entretoise
13 chicane
14 joint torique
Figure 2 — Appareil d’échantillonnage constitué d’une tête de prélèvement équipée d’un
manchon pour retenir les mousses de polyuréthane
3 3
4.2.1.2 Pompe, ayant un débit volumétrique de 2,7 m /h à 2,8 m /h (45 l/min à 46,7 l/min) dans les
conditions d’échantillonnage.
4 © ISO 2014 – Tous droits réservés
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ISO 16000-31:2014(F)
4.2.1.3 Compteur à gaz
4.2.1.4 Hygromètre
4.2.1.5 Thermomètre
4.2.1.6 Baromètre
NOTE L’échantillonnage des COP à l’aide de ‘dispositifs d’échantillonnage à faible volume’ (mousses de
1)
polyuréthane, par exemple ORBO 1000 ) avec un débit d’échantillonnage de 1 l/min à 5 l/min est uniquement
possible dans les limites spécifiées. L’efficacité d’échantillonnage de ces adsorbants pour particules aéroportées
n’est pas connue (voir la Référence 11]). Ce mode opératoire ne satisfait pas aux exigences d’échantillonnage des
particules. Par conséquent, sa comparabilité d’application avec la méthode décrite dans le présent document doit
être prouvée.
4.2.2 Appareil de preparation des échantillons
4.2.2.1 Appareil en verre, matériel de laboratoire habituel.
4.2.2.2 Extracteur, Soxhlet.
4.2.2.3 Seringues microlitres, 10 µl, 50 µl, et 100 µl.
4.2.3 Matériaux d’échantillonnage et de préparation des échantillons
4.2.3.1 Dichlorométhane et toluène, tous les solvants répertoriés doivent être de pureté suffisante
pour l’analyse des éléments traces.
13 13
4.2.3.2 Étalons internes, C-γ-HCH et C-DDE (voir en 6.1).
4.2.3.3 Filtre en fibres de verre, ∅ 5 cm, sans blanc.
4.2.3.4 Mousse de polyuréthane, ∅ 5 cm, longueur de 2,5 cm, avec faibles contaminations.
Instructions de nettoyage pas à pas pour la mousse de polyuréthane « sortie d’usine »:
1) extraction pendant 24 h avec du méthanol dans l’extracteur Soxhlet;
2) extraction pendant 24 h avec du dichlorométhane dans l’extracteur Soxhlet;
3) extraction pendant 24 h avec du toluène dans l’extracteur Soxhlet;
4) extraction pendant 24 h avec de l’acétone dans l’extracteur Soxhlet.
Instructions de nettoyage pour la mousse de polyuréthane prélevée et extraite:
1) extraction pendant 24 h avec du toluène dans l’extracteur Soxhlet;
2) extraction pendant 24 h avec de l’acétone dans l’extracteur Soxhlet.
Sécher la mousse de polyuréthane dans un dessiccateur sous vide et sous écoulement doux d’azote
ultrapur (provenant de l’évaporation de l’azote liquide) ou dans une étuve de séchage sous vide à 40 °C.
1) ORBO 1000 est l’appellation commerciale d’un produit disponible dans le commerce. Cette information
est donnée par souci de commodité à l’intention des utilisateurs du présent document et ne saurait constituer un
engagement de l’ISO à l’égard de ce produit. Des produits équivalents peuvent être utilisés s’il est démontré qu’ils
conduisent aux mêmes résultats.
© ISO 2014 – Tous droits réservés 5
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ISO 16000-31:2014(F)
Les mousses de polyuréthane peuvent se rétracter pendant l’extraction ou le nettoyage. Veiller à ce
qu’elles restent bien fixées après le nettoyage.
4.3 Échantillonnage
L’enrichissement des substances à analyser présentes dans l’air intérieur est effectué sur un filtre en
fibres de verre et sur de la mousse de polyuréthane tout en appliquant la tête de prélèvement décrite
dans l’ISO 16000-13. Les COP liés aux particules et gazeux sont prélevés de cette manière.
L’étalon interne est appliqué à la mousse de polyuréthane, tandis que 100 µl (pour la LRMS) ou 50 µl
(pour la HRMS), respectivement, de la solution d’étalon interne (voir en 6.1 et 6.2.1) sont injectés dans
différentes zones de la mousse (par exemple, avec une seringue microlitre).
Il convient de préférence d’appliquer l’étalon interne avant l’échantillonnage. Si cela s’avère impossible
dans des cas justifiés, l’étalon interne peut également être dopé avant l’extraction et une note justificative
doit être consignée dans le rapport d’essai.
Au niveau de l’emplacement de mesure, la mousse de polyuréthane est insérée dans la tête de
prélèvement. Le filtre en fibres de verre est placé dans le porte-filtres à l’aide de pinces et est fixé. La tête
de prélèvement est positionnée sur le support de manière à ce que l’air prélevé circule à travers la tête
de prélèvement à la verticale, de bas en haut. L’orifice d’aspiration est situé à 1,2 m à 1,5 m au-dessus du
3
sol. La durée de l’échantillonnage est normalement de 1 h. Le débit volumétrique doit être de 2,7 m /h à
3
2,8 m /h. Il convient que le volume d’échantillonnage prélevé en une heure ne dépasse pas 10 % du taux
de renouvellement d’air. SI ce dernier n’est pas connu, alors le volume d’échantillonnage prélevé en une
heure ne doit pas dépasser 10 % du volume de la pièce. La température ambiante, l’humidité relative de
l’air et la pression atmosphérique doivent être mesurées et consignées immédiatement avant et après
l’échantillonnage. À la fin de l’échantillonnage, la mousse de polyuréthane et le filtre en fibres de verre
sont retirés de la tête de prélèvement et transférés dans des récipients de transport appropriés.
4.4 Préparation des échantillons
L’appareil en verre utilisé est entièrement rincé avec du dichlorométhane (DCM). Si l’appareil en
...
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