ISO 16000-6:2011
(Main)Indoor air — Part 6: Determination of volatile organic compounds in indoor and test chamber air by active sampling on Tenax TA sorbent, thermal desorption and gas chromatography using MS or MS-FID
Indoor air — Part 6: Determination of volatile organic compounds in indoor and test chamber air by active sampling on Tenax TA sorbent, thermal desorption and gas chromatography using MS or MS-FID
ISO 16000-6:2011 specifies a method for determination of volatile organic compounds (VOCs) in indoor air and in air sampled for the determination of the emission of VOCs from building products or materials and other products used in indoor environments using test chambers and test cells. The method uses Tenax TAÒ sorbent with subsequent thermal desorption and gas chromatographic analysis employing a capillary column or columns and a flame ionization detector and/or a mass spectrometric detector. The method is applicable to the measurement of non-polar and slightly polar VOCs at concentrations ranging from sub-micrograms per cubic metre to several milligrams per cubic metre. Using the principles specified in this method, an annex describes how some very volatile compounds and semi-volatile organic compounds can also be analysed.
Air intérieur — Partie 6: Dosage des composés organiques volatils dans l'air intérieur des locaux et chambres d'essai par échantillonnage actif sur le sorbant Tenax TA, désorption thermique et chromatographie en phase gazeuse utilisant MS ou MS-FID
L'ISO 16000-6:2011 spécifie une méthode permettant de doser les composés organiques volatils (COV) dans l'air intérieur et dans l'air échantillonné afin de déterminer l'émission de COV provenant de matériaux de construction à l'aide de chambres d'essai et de cellules d'essai. La méthode utilise du sorbant Tenax TA puis une désorption thermique et une analyse par chromatographie en phase gazeuse utilisant une ou plusieurs colonne(s) capillaire(s) avec détecteur à ionisation de flamme et/ou détecteur à spectrométrie de masse. La méthode s'applique au mesurage des COV non polaires et légèrement polaires à des concentrations allant de quelques nanogrammes par mètre cube à plusieurs milligrammes par mètre cube. À l'aide des principes spécifiés dans la présente méthode, certains composés très volatils et semivolatils peuvent également être analysés.
Notranji zrak - 6. del: Določevanje hlapnih organskih spojin v notranjem zraku in zraku v preskusnih komorah z aktivnim vzorčenjem na sorbentu Tenax TA, termično desorpcijo in plinsko kromatografijo z MS ali MS-FID
Ta del standarda ISO 16000 določa metodo za določevanje hlapnih organskih spojin (VOC) v notranjem zraku in zraku, vzorčenem za določevanje emisij hlapnih organskih spojin iz gradbenih izdelkov ali materialov ter drugih izdelkov, ki se uporabljajo v notranjih okoljih, s preskusnimi komorami in celicami. Metoda uporablja sorbent Tenax TA?1) s poznejšo termično desorpcijo (TD) in analizo[13] s plinsko kromatografijo (GC), pri kateri se uporablja ena kapilarna kolona ali več, plamensko ionizacijski detektor (FID) in/ali masno selektivni (MS) detektor. Metoda se uporablja za merjenje nepolarnih ali rahlo polarnih hlapnih organskih spojin v koncentracijah manjših od mikrogramov na kubični meter do več miligramov na kubični meter. Ob upoštevanju načel iz te metode se lahko analizirajo tudi nekatere zelo hlapne spojine (VVC) in polhlapne organske spojine (SVOC) (glejte dodatek D).
General Information
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Buy Standard
Standards Content (Sample)
SLOVENSKI STANDARD
SIST ISO 16000-6:2012
01-april-2012
1DGRPHãþD
SIST ISO 16000-6:2004
1RWUDQML]UDNGHO 'RORþHYDQMHKODSQLKRUJDQVNLKVSRMLQYQRWUDQMHP]UDNXLQ
]UDNXYSUHVNXVQLKNRPRUDK]DNWLYQLPY]RUþHQMHPQDVRUEHQWX7HQD[7$
WHUPLþQRGHVRUSFLMRLQSOLQVNRNURPDWRJUDILMR]06DOL06),'
Indoor air - Part 6: Determination of volatile organic compounds in indoor and test
chamber air by active sampling on Tenax TA sorbent, thermal desorption and gas
chromatography using MS or MS-FID
Air intérieur -- Partie 6: Dosage des composés organiques volatils dans l'air intérieur des
locaux et chambres d'essai par échantillonnage actif sur le sorbant Tenax TA, désorption
thermique et chromatographie en phase gazeuse utilisant MS ou MS-FID
Ta slovenski standard je istoveten z: ISO 16000-6:2011
ICS:
13.040.20 Kakovost okoljskega zraka Ambient atmospheres
SIST ISO 16000-6:2012 en,fr
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST ISO 16000-6:2012
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SIST ISO 16000-6:2012
INTERNATIONAL ISO
STANDARD 16000-6
Second edition
2011-12-01
Indoor air —
Part 6:
Determination of volatile organic
compounds in indoor and test chamber
air by active sampling on Tenax TA
sorbent, thermal desorption and gas
chromatography using MS or MS-FID
Air intérieur —
Partie 6: Dosage des composés organiques volatils dans l'air intérieur
des locaux et chambres d'essai par échantillonnage actif sur le sorbant
Tenax TA , désorption thermique et chromatographie en phase
gazeuse utilisant MS ou MS-FID
Reference number
ISO 16000-6:2011(E)
©
ISO 2011
---------------------- Page: 3 ----------------------
SIST ISO 16000-6:2012
ISO 16000-6:2011(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2011
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,
electronic or mechanical, including photocopying and microfilm, without permission in writing 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 2011 – All rights reserved
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SIST ISO 16000-6:2012
ISO 16000-6:2011(E)
Contents Page
Foreword . iv
Introduction . vi
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 2
5 Reagents and materials . 2
6 Apparatus . 4
7 Conditioning and storage of sorbent tubes . 6
7.1 Conditioning . 6
7.2 Storage of conditioned sorbent tubes before sampling . 6
8 Sampling . 6
8.1 Indoor air sampling . 6
8.2 Test chamber air sampling . 6
8.3 Sampling volumes . 7
8.4 Storage of loaded samples . 7
8.5 Field blanks . 7
9 Analysis . 7
9.1 General . 7
9.2 Thermal desorption . 8
9.3 Temperature programme . 8
9.4 Analysis of the samples. 8
10 Identification of single VOCs . 8
11 Concentration of analytes in the sampled air . 9
11.1 General . 9
11.2 Volatile organic compounds . 9
11.3 Total volatile organic compounds . 10
11.4 VVOC and SVOC compounds observed outside the TVOC range . 10
12 Performance characteristics . 11
13 Test report . 12
14 Quality control . 12
Annex A (informative) Examples of compounds detected in indoor air and from building products
in test chambers . 13
Annex B (informative) Safe sampling volumes for selected organic vapours sampled on Tenax
TA . 19
Annex C (informative) Storage recovery of solvents on Tenax TA sorbent tubes . 21
Annex D (informative) Determination of very volatile and semi-volatile organic compounds in
conjunction with volatile organic compounds . 23
Bibliography . 28
© ISO 2011 – All rights reserved iii
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SIST ISO 16000-6:2012
ISO 16000-6:2011(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies
(ISO member bodies). The work of preparing International Standards is normally carried out through ISO
technical committees. Each member body interested in a subject for which a technical committee has been
established has the right to be represented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the
International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 16000-6 was prepared by Technical Committee ISO/TC 146, Air quality, Subcommittee SC 6, Indoor air.
This second edition cancels and replaces the first edition (ISO 16000-6:2004), which has been technically
revised.
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 2011 – All rights reserved
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SIST ISO 16000-6:2012
ISO 16000-6:2011(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 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
The following parts are under preparation:
Part 21: Detection and enumeration of moulds — Sampling from materials
Part 27: Determination of settled fibrous dust on surfaces by SEM (scanning electron microscopy)
(direct method)
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 constructions on pollutants and other injurious factors — Inspections
© ISO 2011 – All rights reserved v
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SIST ISO 16000-6:2012
ISO 16000-6:2011(E)
Introduction
ISO 16000-1 establishes 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. Aspects of the determination (sampling and analysis) and the sampling strategy of specific
pollutants or groups of pollutants are specified in the subsequent parts of ISO 16000 (see Foreword).
ISO 16000-5 (dealing with VOC sampling strategy) is a link between ISO 16000-1 (a generic standard
establishing the principles) and this part of ISO 16000, which deals with sampling and analytical
measurements.
[3]–[7]
ISO 16017 (see Clause 2 and Reference [8]) and ISO 12219 also focus on volatile organic compound
(VOC) measurements.
vi © ISO 2011 – All rights reserved
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SIST ISO 16000-6:2012
INTERNATIONAL STANDARD ISO 16000-6:2011(E)
Indoor air —
Part 6:
Determination of volatile organic compounds in indoor and test
chamber air by active sampling on Tenax TA sorbent, thermal
desorption and gas chromatography using MS or MS-FID
1 Scope
This part of ISO 16000 specifies a method for determination of volatile organic compounds (VOCs) in indoor
air and in air sampled for the determination of the emission of VOCs from building products or materials and
other products used in indoor environments using test chambers and test cells. The method uses
1) [13]
Tenax TA sorbent with subsequent thermal desorption (TD) and gas chromatographic (GC) analysis
employing a capillary column or columns and a flame ionization detector (FID) and/or a mass spectrometric
(MS) detector.
The method is applicable to the measurement of non-polar and slightly polar VOCs at concentrations ranging
from sub-micrograms per cubic metre to several milligrams per cubic metre. Using the principles specified in
this method, some very volatile compounds (VVOC) and semi-volatile organic compounds (SVOC) can also
be analysed (see Annex D).
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 16000-1, Indoor air — Part 1: General aspects of sampling strategy
ISO 16017-1:2000, Indoor, ambient and workplace air — Sampling and analysis of volatile organic
compounds by sorbent tube/thermal desorption/capillary gas chromatography — Part 1: Pumped sampling
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
semi-volatile organic compound
SVOC
organic compound whose boiling point is in the range from (240 °C to 260 °C) to (380 °C to 400 °C)
[14]
NOTE 1 This classification has been defined by the World Health Organization .
1) Tenax TA is the trade name of a product supplied by Buchem. 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 2011 – All rights reserved 1
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SIST ISO 16000-6:2012
ISO 16000-6:2011(E)
NOTE 2 Boiling points of some compounds are difficult or impossible to determine because they decompose before
they boil at atmospheric pressure. Vapour pressure is another criterion for classification of compound volatility that may be
[15]
used for classification of organic chemicals .
3.2
volatile organic compound
VOC
organic compound whose boiling point is in the range from (50 °C to 100 °C) to (240 °C to 260 °C)
[14]
NOTE 1 This classification has been defined by the World Health Organization .
NOTE 2 Boiling points of some compounds are difficult or impossible to determine because they decompose before
they boil at atmospheric pressure. Vapour pressure is another criterion for classification of compound volatility that may be
[15]
used for classification of organic chemicals .
3.3
very volatile organic compound
VVOC
organic compound whose boiling point is in the range from 0 °C to (50 °C to 100 °C)
[14]
NOTE 1 This classification has been defined by the World Health Organization .
NOTE 2 Boiling points of some compounds are difficult or impossible to determine because they decompose before
they boil at atmospheric pressure. Vapour pressure is another criterion for classification of compound volatility that may be
[15]
used for classification of organic chemicals .
3.4
total volatile organic compounds
TVOCs
sum of volatile organic compounds, sampled on Tenax TA , which elute between and including n-hexane and
n-hexadecane on a non-polar capillary column, detected with a flame ionization detector (TVOC-FID) or mass
spectrometric detector (TVOC-MS), and quantified by converting the total area of the chromatogram in that
analytical window to a nominal mass using the chromatographic response factor for toluene (toluene
equivalents)
NOTE While this part of ISO 16000 specifies the determination of individual VOCs, it is common in practice to
generate a single concentration value to characterize the total amount of VOCs present in the air. This value is called the
TVOC value (see 11.3 and Clause 13). It should be emphasized that the TVOC value so obtained depends on the
sampling and analytical methods used, and therefore should be interpreted taking into account the full description of these
methods.
4 Principle
A measured volume of sample air is collected from room air, an emission test chamber (see ISO 16000-9) or
an emission test cell (see ISO 16000-10) by drawing through one (or more) sorbent tube containing
Tenax TA sorbent. Volatile organic compounds (VOCs) are retained by the sorbent tube, and the
compounds are subsequently analysed in the laboratory. The collected VOCs are desorbed by heat and
transferred under inert carrier gas via a cold trap or sorbent trap into a gas chromatograph equipped with a
capillary column or columns and a flame ionization detector and/or a mass spectrometric detector.
5 Reagents and materials
5.1 Volatile organic compounds for calibration, of chromatographic quality.
5.2 Dilution solvent, for preparing calibration blend solution for liquid spiking, of chromatographic quality,
free from compounds co-eluting with the compound(s) of interest (5.1).
NOTE It is in most cases beneficial to use dilution solvent that is considerably more volatile than the VOCs to be
analysed. Methanol most commonly fulfils this criterion. Health and safety data for organic compounds are given, for
[24]
example, in International Chemical Safety Cards (ICSCs) .
2 © ISO 2011 – All rights reserved
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SIST ISO 16000-6:2012
ISO 16000-6:2011(E)
5.3 Tenax TA , particle size 0,18 mm to 0,60 mm (30 mesh to 80 mesh).
Tenax TA is a porous polymer based on 2,6-diphenyleneoxide. Manufactured Tenax TA contains quantities
of impurities, which shall be removed before using it for VOC sampling. Perform cleaning by thermal
conditioning the Tenax TA under a flow of pure carrier gas. Select cleaning conditions so that no degradation
of the polymer occurs, e.g. at a temperature of 300 °C for 10 h using a carrier gas flow rate of 50 ml/min to
100 ml/min for packed sampling tubes. Pack pre-cleaned Tenax TA into sampling tubes that are tightly
sealed and store in a closed, emission-free container. Check the success of the cleaning procedure by
performing an analysis of the cleaned sorbent.
NOTE Pre-packed, conditioned (cleaned) and capped sorbent tubes are available commercially.
5.4 Standard atmospheres, of known concentrations of the compound(s) of interest, prepared by a
[1] [2]
recognized procedure. Methods specified in ISO 6141 and the appropriate part of ISO 6145 are suitable.
3
Prepare standard atmospheres equivalent to about 100 µg/m . If the procedure is not applied under
conditions that allow the establishment of full traceability of the generated concentrations to primary standards
of mass and/or volume, or if the chemical inertness of the generation system cannot be guaranteed, the
concentrations shall be confirmed using an independent procedure.
5.5 Standard sorbent tubes, loaded by spiking from standard atmospheres (5.4), prepared by passing an
accurately known volume of the standard atmosphere through the sorbent tube, e.g. by means of a pump.
The volume of atmosphere sampled shall not exceed the breakthrough volume of the analyte-sorbent
combination. After loading, disconnect and seal the tube. Prepare fresh standards with each batch of samples.
For indoor air and test chamber air, load sorbent tubes with e.g. 100 ml, 200 ml, 400 ml, 1 l, 2 l, 4 l or 10 l of
3
the 100 µg/m standard atmosphere selected.
5.6 Calibration blend solutions for liquid spiking.
5.6.1 General. The stability and safe storage times of calibration blend solutions shall be determined. Fresh
standard solutions shall be prepared accordingly or if there is evidence of deterioration, e.g. reactions
between alcohols and ketones. Appropriate calibration solution concentrations vary depending upon expected
target analyte levels in each batch of samples. Examples of solution preparation for a range of applications
are given in 5.6.2 to 5.6.6.
5.6.2 Solution containing approximately 10 mg/ml of each liquid component. Introduce 50 ml of
dilution solvent into a 100 ml volumetric flask. Accurately weigh approximately 1 g of substance or substances
of interest into a 100 ml volumetric flask, starting with the least volatile substance. Make up to 100 ml with
dilution solvent, stopper and shake to mix.
5.6.3 Solution containing approximately 1 000 µg/ml of each liquid component. Introduce 50 ml of
dilution solvent into a 100 ml volumetric flask. Add 10 ml of solution 5.6.2. Make up to 100 ml with dilution
solvent, stopper and shake to mix.
5.6.4 Solution containing approximately 100 µg/ml of each liquid component. Introduce 50 ml of
dilution solvent into a 100 ml volumetric flask. Add 10 ml of solution 5.6.3. Make up to 100 ml with dilution
solvent, stopper and shake to mix.
5.6.5 Solution containing approximately 10 µg/ml of each liquid component. Introduce 50 ml of dilution
solvent into a 100 ml volumetric flask. Add 10 ml of solution 5.6.4. Make up to 100 ml with dilution solvent,
stopper and shake to mix.
5.6.6 Solution containing approximately 1 µg/ml of each liquid component. Introduce 50 ml of dilution
solvent into a 100 ml volumetric flask. Add 10 ml of solution 5.6.5. Make up to 100 ml with dilution solvent,
stopper and shake to mix.
5.7 Standard sorbent tubes, loaded by spiking, prepared by injecting aliquots of standard solutions on to
clean sorbent tubes.
© ISO 2011 – All rights reserved 3
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SIST ISO 16000-6:2012
ISO 16000-6:2011(E)
The sampling end of a sorbent tube is fitted to the unheated injection unit of the gas chromatograph (GC)
(6.10) through which inert purge gas is passed at 100 ml/min, and a 1 µl to 5 µl aliquot of an appropriate
standard solution is injected through the septum. After 5 min, the tube is disconnected and sealed. Prepare
fresh standard tubes with each batch of samples.
Introducing liquid standards on to sorbent tubes via a GC injector is considered the optimum approach to
liquid standard introduction, as components reach the sorbent bed in the vapour phase. Alternatively, liquid
standards may be introduced directly on to the sorbent bed using a syringe (6.3).
Calibration mixtures should be prepared in controlled ambient temperature conditions. Before use, temper the
solutions accordingly.
NOTE 1 When preparing standard tubes containing SVOC analytes, efficient transfer is enhanced if the configuration
of injector allows the tip of the syringe to make gentle contact with the sorbent retaining mechanism (e.g. gauze or frit)
within the tube.
NOTE 2 Standard tubes containing VVOCs are more typically prepared either from standard atmospheres (see 5.4 and
5.5) or from concentrated gas standards sourced commercially. It is appropriate for concentrated gas standards to be
introduced to the sampling end of sorbent tubes in a stream of carrier gas via an unheated GC injector.
NOTE 3 If standard tubes are being prepared by introducing aliquots from more than one standard solution or gas, it is
appropriate first to introduce the standard containing higher boiling components and to introduce the lightest components
last. This minimizes risk of analyte breakthrough during the standard tube loading process.
5.8 Commercial, preloaded standard tubes, certified, are available and can be used for establishing
analytical quality control and for routine calibration.
5.9 Inert carrier gas, e.g. He, Ar, N . The purity of the carrier gas should permit the detection of an
2
injection of 0,5 ng of toluene.
CAUTION — The quality of the carrier gas is of great importance, as contaminants possibly contained
in the gases are enriched in the cold trap together with the substances to be analysed.
6 Apparatus
Ordinary laboratory apparatus and in particular the following.
6.1 Sorbent tubes, of stainless steel or glass, containing at least 200 mg of Tenax TA sorbent (5.3),
with metal screw caps and polytetrafluoroethene (PTFE) ferrules.
Tubes with outside diameter of 6,4 mm (0.25 inch), inside diameter of 5 mm, and of length 89 mm (3.5 inch)
fulfil the requirement and are used in many commercial thermal desorbers. Use deactivated glass wool or
other suitable mechanism, e.g. stainless steel frit, to retain the sorbent in the tube.
NOTE 1 The unit inch is not allowed in ISO documents; inch equivalents are given for information only.
Pre-cleaned sorbent tubes containing Tenax TA are available commercially. Alternatively, sorbent tubes can
be filled in the laboratory as follows.
Weigh the appropriate amount of adsorbent, using no less than 200 mg of sorbent per tube to maintain the
sorption capacity. To pack the tube, insert a plug of deactivated glass wool or a stainless steel gauze into one
end of the tube. Transfer the adsorbent into the tube, assisted by suction if desired. Place an additional plug
or gauze after the sorbent to retain it in the tube.
NOTE 2 The determination of breakthrough volume is specified in ISO 16017-1:2000, Annex B. Breakthrough volumes
are proportional to the dimensions of the sampling tube and quantity of sorbent. As an approximate measure, doubling the
bed length while tube diameter is kept constant doubles the safe sampling volume (SSV).
4 © ISO 2011 – All rights reserved
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SIST ISO 16000-6:2012
ISO 16000-6:2011(E)
6.2 Sorbent tube unions. For sampling, two sorbent tubes connected in series using metal screw-cap
couplings with PTFE ferrules.
6.3 Precision syringes, readable to at least 0,1 µl.
[11] [10]
6.4 Sampling pump, fulfilling the requirements of EN 1232 or ASTM D3686 .
6.5 Tubing, of polyethylene (PE) or PTFE, of appropriate diameter, used to ensure a leak-proof fit to both
pump and sample tube.
Sampling tubes shall not be used with plastic tubing upstream of the sorbent. Interferences from the tubing
can introduce contaminants.
6.6 Flow meter calibrator. Bubble meter or other suitable device for gas flow calibration.
6.7 Gas chromatographic (GC) system, fitted with a flame ionization detector and/or mass spectrometric
detector capable of detecting an injection of at least 1 ng of toluene with a signal-to-noise ratio of at least
5 to 1.
6.8 Capillary column. A suitable GC capillary column is selected for separation of analytes in the sample.
Bonded 100 % dimethylpolysiloxane columns of 30 m to 60 m, internal diameter 0,25 mm to 0,32 mm and
phase thickness 0,25 µm to 0,5 µm are examples of columns proven to be suitable for VOC analysis of indoor
air, emission test chamber (in accordance with ISO 16000-9) air, and emission test cell (in accordance with
ISO 16000-10) air.
)
2
NOTE A dimethylpolysiloxane column, e.g. an HP-
...
INTERNATIONAL ISO
STANDARD 16000-6
Second edition
2011-12-01
Indoor air —
Part 6:
Determination of volatile organic
compounds in indoor and test chamber
air by active sampling on Tenax TA
sorbent, thermal desorption and gas
chromatography using MS or MS-FID
Air intérieur —
Partie 6: Dosage des composés organiques volatils dans l'air intérieur
des locaux et chambres d'essai par échantillonnage actif sur le sorbant
Tenax TA , désorption thermique et chromatographie en phase
gazeuse utilisant MS ou MS-FID
Reference number
ISO 16000-6:2011(E)
©
ISO 2011
---------------------- Page: 1 ----------------------
ISO 16000-6:2011(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2011
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,
electronic or mechanical, including photocopying and microfilm, without permission in writing 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 2011 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 16000-6:2011(E)
Contents Page
Foreword . iv
Introduction . vi
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 2
5 Reagents and materials . 2
6 Apparatus . 4
7 Conditioning and storage of sorbent tubes . 6
7.1 Conditioning . 6
7.2 Storage of conditioned sorbent tubes before sampling . 6
8 Sampling . 6
8.1 Indoor air sampling . 6
8.2 Test chamber air sampling . 6
8.3 Sampling volumes . 7
8.4 Storage of loaded samples . 7
8.5 Field blanks . 7
9 Analysis . 7
9.1 General . 7
9.2 Thermal desorption . 8
9.3 Temperature programme . 8
9.4 Analysis of the samples. 8
10 Identification of single VOCs . 8
11 Concentration of analytes in the sampled air . 9
11.1 General . 9
11.2 Volatile organic compounds . 9
11.3 Total volatile organic compounds . 10
11.4 VVOC and SVOC compounds observed outside the TVOC range . 10
12 Performance characteristics . 11
13 Test report . 12
14 Quality control . 12
Annex A (informative) Examples of compounds detected in indoor air and from building products
in test chambers . 13
Annex B (informative) Safe sampling volumes for selected organic vapours sampled on Tenax
TA . 19
Annex C (informative) Storage recovery of solvents on Tenax TA sorbent tubes . 21
Annex D (informative) Determination of very volatile and semi-volatile organic compounds in
conjunction with volatile organic compounds . 23
Bibliography . 28
© ISO 2011 – All rights reserved iii
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ISO 16000-6:2011(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies
(ISO member bodies). The work of preparing International Standards is normally carried out through ISO
technical committees. Each member body interested in a subject for which a technical committee has been
established has the right to be represented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the
International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 16000-6 was prepared by Technical Committee ISO/TC 146, Air quality, Subcommittee SC 6, Indoor air.
This second edition cancels and replaces the first edition (ISO 16000-6:2004), which has been technically
revised.
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 2011 – All rights reserved
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ISO 16000-6:2011(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 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
The following parts are under preparation:
Part 21: Detection and enumeration of moulds — Sampling from materials
Part 27: Determination of settled fibrous dust on surfaces by SEM (scanning electron microscopy)
(direct method)
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 constructions on pollutants and other injurious factors — Inspections
© ISO 2011 – All rights reserved v
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ISO 16000-6:2011(E)
Introduction
ISO 16000-1 establishes 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. Aspects of the determination (sampling and analysis) and the sampling strategy of specific
pollutants or groups of pollutants are specified in the subsequent parts of ISO 16000 (see Foreword).
ISO 16000-5 (dealing with VOC sampling strategy) is a link between ISO 16000-1 (a generic standard
establishing the principles) and this part of ISO 16000, which deals with sampling and analytical
measurements.
[3]–[7]
ISO 16017 (see Clause 2 and Reference [8]) and ISO 12219 also focus on volatile organic compound
(VOC) measurements.
vi © ISO 2011 – All rights reserved
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INTERNATIONAL STANDARD ISO 16000-6:2011(E)
Indoor air —
Part 6:
Determination of volatile organic compounds in indoor and test
chamber air by active sampling on Tenax TA sorbent, thermal
desorption and gas chromatography using MS or MS-FID
1 Scope
This part of ISO 16000 specifies a method for determination of volatile organic compounds (VOCs) in indoor
air and in air sampled for the determination of the emission of VOCs from building products or materials and
other products used in indoor environments using test chambers and test cells. The method uses
1) [13]
Tenax TA sorbent with subsequent thermal desorption (TD) and gas chromatographic (GC) analysis
employing a capillary column or columns and a flame ionization detector (FID) and/or a mass spectrometric
(MS) detector.
The method is applicable to the measurement of non-polar and slightly polar VOCs at concentrations ranging
from sub-micrograms per cubic metre to several milligrams per cubic metre. Using the principles specified in
this method, some very volatile compounds (VVOC) and semi-volatile organic compounds (SVOC) can also
be analysed (see Annex D).
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 16000-1, Indoor air — Part 1: General aspects of sampling strategy
ISO 16017-1:2000, Indoor, ambient and workplace air — Sampling and analysis of volatile organic
compounds by sorbent tube/thermal desorption/capillary gas chromatography — Part 1: Pumped sampling
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
semi-volatile organic compound
SVOC
organic compound whose boiling point is in the range from (240 °C to 260 °C) to (380 °C to 400 °C)
[14]
NOTE 1 This classification has been defined by the World Health Organization .
1) Tenax TA is the trade name of a product supplied by Buchem. 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 2011 – All rights reserved 1
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ISO 16000-6:2011(E)
NOTE 2 Boiling points of some compounds are difficult or impossible to determine because they decompose before
they boil at atmospheric pressure. Vapour pressure is another criterion for classification of compound volatility that may be
[15]
used for classification of organic chemicals .
3.2
volatile organic compound
VOC
organic compound whose boiling point is in the range from (50 °C to 100 °C) to (240 °C to 260 °C)
[14]
NOTE 1 This classification has been defined by the World Health Organization .
NOTE 2 Boiling points of some compounds are difficult or impossible to determine because they decompose before
they boil at atmospheric pressure. Vapour pressure is another criterion for classification of compound volatility that may be
[15]
used for classification of organic chemicals .
3.3
very volatile organic compound
VVOC
organic compound whose boiling point is in the range from 0 °C to (50 °C to 100 °C)
[14]
NOTE 1 This classification has been defined by the World Health Organization .
NOTE 2 Boiling points of some compounds are difficult or impossible to determine because they decompose before
they boil at atmospheric pressure. Vapour pressure is another criterion for classification of compound volatility that may be
[15]
used for classification of organic chemicals .
3.4
total volatile organic compounds
TVOCs
sum of volatile organic compounds, sampled on Tenax TA , which elute between and including n-hexane and
n-hexadecane on a non-polar capillary column, detected with a flame ionization detector (TVOC-FID) or mass
spectrometric detector (TVOC-MS), and quantified by converting the total area of the chromatogram in that
analytical window to a nominal mass using the chromatographic response factor for toluene (toluene
equivalents)
NOTE While this part of ISO 16000 specifies the determination of individual VOCs, it is common in practice to
generate a single concentration value to characterize the total amount of VOCs present in the air. This value is called the
TVOC value (see 11.3 and Clause 13). It should be emphasized that the TVOC value so obtained depends on the
sampling and analytical methods used, and therefore should be interpreted taking into account the full description of these
methods.
4 Principle
A measured volume of sample air is collected from room air, an emission test chamber (see ISO 16000-9) or
an emission test cell (see ISO 16000-10) by drawing through one (or more) sorbent tube containing
Tenax TA sorbent. Volatile organic compounds (VOCs) are retained by the sorbent tube, and the
compounds are subsequently analysed in the laboratory. The collected VOCs are desorbed by heat and
transferred under inert carrier gas via a cold trap or sorbent trap into a gas chromatograph equipped with a
capillary column or columns and a flame ionization detector and/or a mass spectrometric detector.
5 Reagents and materials
5.1 Volatile organic compounds for calibration, of chromatographic quality.
5.2 Dilution solvent, for preparing calibration blend solution for liquid spiking, of chromatographic quality,
free from compounds co-eluting with the compound(s) of interest (5.1).
NOTE It is in most cases beneficial to use dilution solvent that is considerably more volatile than the VOCs to be
analysed. Methanol most commonly fulfils this criterion. Health and safety data for organic compounds are given, for
[24]
example, in International Chemical Safety Cards (ICSCs) .
2 © ISO 2011 – All rights reserved
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ISO 16000-6:2011(E)
5.3 Tenax TA , particle size 0,18 mm to 0,60 mm (30 mesh to 80 mesh).
Tenax TA is a porous polymer based on 2,6-diphenyleneoxide. Manufactured Tenax TA contains quantities
of impurities, which shall be removed before using it for VOC sampling. Perform cleaning by thermal
conditioning the Tenax TA under a flow of pure carrier gas. Select cleaning conditions so that no degradation
of the polymer occurs, e.g. at a temperature of 300 °C for 10 h using a carrier gas flow rate of 50 ml/min to
100 ml/min for packed sampling tubes. Pack pre-cleaned Tenax TA into sampling tubes that are tightly
sealed and store in a closed, emission-free container. Check the success of the cleaning procedure by
performing an analysis of the cleaned sorbent.
NOTE Pre-packed, conditioned (cleaned) and capped sorbent tubes are available commercially.
5.4 Standard atmospheres, of known concentrations of the compound(s) of interest, prepared by a
[1] [2]
recognized procedure. Methods specified in ISO 6141 and the appropriate part of ISO 6145 are suitable.
3
Prepare standard atmospheres equivalent to about 100 µg/m . If the procedure is not applied under
conditions that allow the establishment of full traceability of the generated concentrations to primary standards
of mass and/or volume, or if the chemical inertness of the generation system cannot be guaranteed, the
concentrations shall be confirmed using an independent procedure.
5.5 Standard sorbent tubes, loaded by spiking from standard atmospheres (5.4), prepared by passing an
accurately known volume of the standard atmosphere through the sorbent tube, e.g. by means of a pump.
The volume of atmosphere sampled shall not exceed the breakthrough volume of the analyte-sorbent
combination. After loading, disconnect and seal the tube. Prepare fresh standards with each batch of samples.
For indoor air and test chamber air, load sorbent tubes with e.g. 100 ml, 200 ml, 400 ml, 1 l, 2 l, 4 l or 10 l of
3
the 100 µg/m standard atmosphere selected.
5.6 Calibration blend solutions for liquid spiking.
5.6.1 General. The stability and safe storage times of calibration blend solutions shall be determined. Fresh
standard solutions shall be prepared accordingly or if there is evidence of deterioration, e.g. reactions
between alcohols and ketones. Appropriate calibration solution concentrations vary depending upon expected
target analyte levels in each batch of samples. Examples of solution preparation for a range of applications
are given in 5.6.2 to 5.6.6.
5.6.2 Solution containing approximately 10 mg/ml of each liquid component. Introduce 50 ml of
dilution solvent into a 100 ml volumetric flask. Accurately weigh approximately 1 g of substance or substances
of interest into a 100 ml volumetric flask, starting with the least volatile substance. Make up to 100 ml with
dilution solvent, stopper and shake to mix.
5.6.3 Solution containing approximately 1 000 µg/ml of each liquid component. Introduce 50 ml of
dilution solvent into a 100 ml volumetric flask. Add 10 ml of solution 5.6.2. Make up to 100 ml with dilution
solvent, stopper and shake to mix.
5.6.4 Solution containing approximately 100 µg/ml of each liquid component. Introduce 50 ml of
dilution solvent into a 100 ml volumetric flask. Add 10 ml of solution 5.6.3. Make up to 100 ml with dilution
solvent, stopper and shake to mix.
5.6.5 Solution containing approximately 10 µg/ml of each liquid component. Introduce 50 ml of dilution
solvent into a 100 ml volumetric flask. Add 10 ml of solution 5.6.4. Make up to 100 ml with dilution solvent,
stopper and shake to mix.
5.6.6 Solution containing approximately 1 µg/ml of each liquid component. Introduce 50 ml of dilution
solvent into a 100 ml volumetric flask. Add 10 ml of solution 5.6.5. Make up to 100 ml with dilution solvent,
stopper and shake to mix.
5.7 Standard sorbent tubes, loaded by spiking, prepared by injecting aliquots of standard solutions on to
clean sorbent tubes.
© ISO 2011 – All rights reserved 3
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ISO 16000-6:2011(E)
The sampling end of a sorbent tube is fitted to the unheated injection unit of the gas chromatograph (GC)
(6.10) through which inert purge gas is passed at 100 ml/min, and a 1 µl to 5 µl aliquot of an appropriate
standard solution is injected through the septum. After 5 min, the tube is disconnected and sealed. Prepare
fresh standard tubes with each batch of samples.
Introducing liquid standards on to sorbent tubes via a GC injector is considered the optimum approach to
liquid standard introduction, as components reach the sorbent bed in the vapour phase. Alternatively, liquid
standards may be introduced directly on to the sorbent bed using a syringe (6.3).
Calibration mixtures should be prepared in controlled ambient temperature conditions. Before use, temper the
solutions accordingly.
NOTE 1 When preparing standard tubes containing SVOC analytes, efficient transfer is enhanced if the configuration
of injector allows the tip of the syringe to make gentle contact with the sorbent retaining mechanism (e.g. gauze or frit)
within the tube.
NOTE 2 Standard tubes containing VVOCs are more typically prepared either from standard atmospheres (see 5.4 and
5.5) or from concentrated gas standards sourced commercially. It is appropriate for concentrated gas standards to be
introduced to the sampling end of sorbent tubes in a stream of carrier gas via an unheated GC injector.
NOTE 3 If standard tubes are being prepared by introducing aliquots from more than one standard solution or gas, it is
appropriate first to introduce the standard containing higher boiling components and to introduce the lightest components
last. This minimizes risk of analyte breakthrough during the standard tube loading process.
5.8 Commercial, preloaded standard tubes, certified, are available and can be used for establishing
analytical quality control and for routine calibration.
5.9 Inert carrier gas, e.g. He, Ar, N . The purity of the carrier gas should permit the detection of an
2
injection of 0,5 ng of toluene.
CAUTION — The quality of the carrier gas is of great importance, as contaminants possibly contained
in the gases are enriched in the cold trap together with the substances to be analysed.
6 Apparatus
Ordinary laboratory apparatus and in particular the following.
6.1 Sorbent tubes, of stainless steel or glass, containing at least 200 mg of Tenax TA sorbent (5.3),
with metal screw caps and polytetrafluoroethene (PTFE) ferrules.
Tubes with outside diameter of 6,4 mm (0.25 inch), inside diameter of 5 mm, and of length 89 mm (3.5 inch)
fulfil the requirement and are used in many commercial thermal desorbers. Use deactivated glass wool or
other suitable mechanism, e.g. stainless steel frit, to retain the sorbent in the tube.
NOTE 1 The unit inch is not allowed in ISO documents; inch equivalents are given for information only.
Pre-cleaned sorbent tubes containing Tenax TA are available commercially. Alternatively, sorbent tubes can
be filled in the laboratory as follows.
Weigh the appropriate amount of adsorbent, using no less than 200 mg of sorbent per tube to maintain the
sorption capacity. To pack the tube, insert a plug of deactivated glass wool or a stainless steel gauze into one
end of the tube. Transfer the adsorbent into the tube, assisted by suction if desired. Place an additional plug
or gauze after the sorbent to retain it in the tube.
NOTE 2 The determination of breakthrough volume is specified in ISO 16017-1:2000, Annex B. Breakthrough volumes
are proportional to the dimensions of the sampling tube and quantity of sorbent. As an approximate measure, doubling the
bed length while tube diameter is kept constant doubles the safe sampling volume (SSV).
4 © ISO 2011 – All rights reserved
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ISO 16000-6:2011(E)
6.2 Sorbent tube unions. For sampling, two sorbent tubes connected in series using metal screw-cap
couplings with PTFE ferrules.
6.3 Precision syringes, readable to at least 0,1 µl.
[11] [10]
6.4 Sampling pump, fulfilling the requirements of EN 1232 or ASTM D3686 .
6.5 Tubing, of polyethylene (PE) or PTFE, of appropriate diameter, used to ensure a leak-proof fit to both
pump and sample tube.
Sampling tubes shall not be used with plastic tubing upstream of the sorbent. Interferences from the tubing
can introduce contaminants.
6.6 Flow meter calibrator. Bubble meter or other suitable device for gas flow calibration.
6.7 Gas chromatographic (GC) system, fitted with a flame ionization detector and/or mass spectrometric
detector capable of detecting an injection of at least 1 ng of toluene with a signal-to-noise ratio of at least
5 to 1.
6.8 Capillary column. A suitable GC capillary column is selected for separation of analytes in the sample.
Bonded 100 % dimethylpolysiloxane columns of 30 m to 60 m, internal diameter 0,25 mm to 0,32 mm and
phase thickness 0,25 µm to 0,5 µm are examples of columns proven to be suitable for VOC analysis of indoor
air, emission test chamber (in accordance with ISO 16000-9) air, and emission test cell (in accordance with
ISO 16000-10) air.
)
2
NOTE A dimethylpolysiloxane column, e.g. an HP-1 column, does not separate 3-carene from 2-ethyl-1-hexanol
with certain oven programmes, nor does it separate m- and p-xylenes.
6.9 Thermal desorption apparatus, for the two-stage thermal desorption of the sorbent tubes and transfer
of desorbed vapours via an inert gas flow into a GC.
A typical apparatus contains a mechanism for holding the tubes to be desorbed while they are heated and
purged simultaneously with inert carrier gas. The desorption temperature and time are adjustable, as is the
carrier gas flow rate. The apparatus may also incorporate additional features, such as automatic sample-tube
loading, leak testing, and a cold trap or other suitable device to concentrate the desorbed sample. The
desorbed sample, contained in the purge gas, is routed to the gas chromatograph and capillary column via a
heated transfer line.
6.10 Injection facility for preparing standards by liquid spiking (optional). A conventional gas
chromatographic injection unit or equivalent device may be used for preparing calibration standards. This can
be used in situ, or it can be mounted separately. The injector should be unheated to eliminate risk of heat
transfer to the tube and associated risk of analyte breakthrough. The back of the injection unit should be
adapted if necessary to fit the sample tube. This can be done conveniently by means of compression coupling
with an O-ring seal.
NOTE W
...
NORME ISO
INTERNATIONALE 16000-6
Deuxième édition
2011-12-01
Air intérieur —
Partie 6:
Dosage des composés organiques
volatils dans l'air intérieur des locaux et
chambres d'essai par échantillonnage
actif sur le sorbant Tenax TA ,
désorption thermique et chromatographie
en phase gazeuse utilisant MS ou MS-FID
Indoor air —
Part 6: Determination of volatile organic compounds in indoor and test
chamber air by active sampling on Tenax TA sorbent, thermal
desorption and gas chromatography using MS or MS-FID
Numéro de référence
ISO 16000-6:2011(F)
©
ISO 2011
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ISO 16000-6:2011(F)
DOCUMENT PROTÉGÉ PAR COPYRIGHT
© ISO 2011
Droits de reproduction réservés. Sauf prescription différente, 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 et les microfilms, sans l'accord écrit
de l'ISO à l'adresse ci-après ou du comité membre de l'ISO dans le pays du demandeur.
ISO copyright office
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Web www.iso.org
Publié en Suisse
ii © ISO 2011 – Tous droits réservés
---------------------- Page: 2 ----------------------
ISO 16000-6:2011(F)
Sommaire Page
Avant-propos . iv
Introduction . vi
1 Domaine d'application . 1
2 Références normatives . 1
3 Termes et définitions . 2
4 Principe . 2
5 Réactifs et matériaux . 3
6 Appareillage . 5
7 Conditionnement et conservation des tubes à sorbant . 6
7.1 Conditionnement . 6
7.2 Conservation des tubes à sorbant conditionnés avant échantillonnage . 6
8 Échantillonnage . 7
8.1 Échantillonnage d'air intérieur . 7
8.2 Échantillonnage d'air en chambre d'essai . 7
8.3 Volumes de prélèvement . 7
8.4 Conservation des échantillons chargés . 8
8.5 Échantillons blancs . 8
9 Analyse . 8
9.1 Généralités . 8
9.2 Désorption thermique . 8
9.3 Programmation des températures . 9
9.4 Analyse des échantillons . 9
10 Identification de COV individuels. 9
11 Concentration des analytes dans l'air échantillonné . 10
11.1 Généralités . 10
11.2 Composés organiques volatils . 10
11.3 Composés organiques volatils totaux . 11
11.4 Composés de COTV et de COSV observés en dehors de la gamme de COVT . 11
12 Caractéristiques de performance . 12
13 Rapport d'essai . 13
14 Contrôle qualité. 13
Annexe A (informative) Exemples de composés détectés dans l'air intérieur et émanant des
produits de construction dans les chambres d'essai . 15
Annexe B (informative) Volumes limites de prélèvement des vapeurs organiques sélectionnées et
®
échantillonnées sur Tenax TA . 21
Annexe C (informative) Récupération des solvants après conservation dans des tubes à sorbant
®
Tenax TA . 23
Annexe D (informative) Dosage des composés organiques très volatils et semi-volatils
parallèlement aux composés organiques volatils. 25
Bibliographie . 31
© ISO 2011 – Tous droits réservés iii
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ISO 16000-6:2011(F)
Avant-propos
L'ISO (Organisation internationale de normalisation) est une fédération mondiale d'organismes nationaux de
normalisation (comités membres de l'ISO). L'élaboration des Normes internationales est en général confiée
aux comités techniques de l'ISO. Chaque comité membre intéressé par une étude a le droit de faire partie du
comité technique créé à cet effet. Les organisations internationales, gouvernementales et non
gouvernementales, en liaison avec l'ISO participent également aux travaux. L'ISO collabore étroitement avec
la Commission électrotechnique internationale (CEI) en ce qui concerne la normalisation électrotechnique.
Les Normes internationales sont rédigées conformément aux règles données dans les Directives ISO/CEI,
Partie 2.
La tâche principale des comités techniques est d'élaborer les Normes internationales. Les projets de Normes
internationales adoptés par les comités techniques sont soumis aux comités membres pour vote. Leur
publication comme Normes internationales requiert l'approbation de 75 % au moins des comités membres
votants.
L'attention est appelée sur le fait que certains des éléments du présent document peuvent faire l'objet de
droits de propriété intellectuelle ou de droits analogues. L'ISO ne saurait être tenue pour responsable de ne
pas avoir identifié de tels droits de propriété et averti de leur existence.
L'ISO 16000-6 a été élaborée par le comité technique ISO/TC 146, Qualité de l'air, sous-comité SC 6, Air
intérieur.
Cette deuxième édition annule et remplace la première édition (ISO 16000-6:2004), qui a fait l'objet d'une
révision technique.
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 chambres d'essai
®
par échantillonnage actif sur le sorbant Tenax TA , désorption thermique et chromatographie en phase
gazeuse utilisant MS ou 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
iv © ISO 2011 – Tous droits réservés
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ISO 16000-6:2011(F)
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)/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 )
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 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 (sauf formaldéhyde) par des matériaux de construction sorptifs
Partie 25: Dosage de l'émission de composés organiques semi-volatils des produits de construction —
Méthode de la micro-chambre
Partie 26: Stratégie d'échantillonnage du dioxyde de carbone (CO )
2
Partie 28: Détermination des émissions d'odeurs des produits de construction au moyen de chambres
d'essai
Les parties suivantes sont en cours d'élaboration:
Partie 21: Détection et dénombrement des moisissures — Échantillonnage à partir de matériaux
Partie 27: Détermination de la poussière fibreuse déposée sur les surfaces par microscopie électronique
à balayage (MEB) (méthode directe)
Partie 29: Méthodes d'essai pour détecteurs de composés organiques volatils (COV)
Partie 30: Essai sensoriel de l'air intérieur
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
© ISO 2011 – Tous droits réservés v
---------------------- Page: 5 ----------------------
ISO 16000-6:2011(F)
Introduction
L'ISO 16000-1 établit les exigences générales relatives au mesurage des polluants de l'air intérieur et les
conditions qu'il est important de respecter avant ou pendant l'échantillonnage de polluants isolés ou de
groupes de polluants. Les détails relatifs au dosage (échantillonnage et analyse) ainsi que la stratégie
d'échantillonnage des polluants ou des groupes spécifiques de polluants sont spécifiés dans les autres parties
de l'ISO 16000 (voir l'Avant-propos).
L'ISO 16000-5 (traitant de la stratégie d'échantillonnage des COV) est un lien entre l'ISO 16000-1 (une norme
générique établissant les principes) et la présente partie de l'ISO 16000 traitant de l'échantillonnage et des
mesurages analytiques.
[3]–[7]
L'ISO 16017 (voir Article 2 et Référence [8]) et l'ISO 12219 portent également sur les mesurages relatifs
aux composés organiques volatils (COV).
vi © ISO 2011 – Tous droits réservés
---------------------- Page: 6 ----------------------
NORME INTERNATIONALE ISO 16000-6:2011(F)
Air intérieur —
Partie 6:
Dosage des composés organiques volatils dans l'air intérieur
des locaux et chambres d'essai par échantillonnage actif sur le
sorbant Tenax TA , désorption thermique et chromatographie
en phase gazeuse utilisant MS ou MS-FID
1 Domaine d'application
La présente partie de l'ISO 16000 spécifie une méthode permettant de doser les composés organiques
volatils (COV) dans l'air intérieur et dans l'air échantillonné afin de déterminer l'émission de COV provenant de
matériaux de construction à l'aide de chambres d'essai et de cellules d'essai. La méthode utilise du sorbant
®1)
Tenax TA puis une désorption thermique (TD) et une analyse par chromatographie en phase gazeuse
[13]
(GC) utilisant une ou plusieurs colonne(s) capillaire(s) avec détecteur à ionisation de flamme (FID) et/ou
détecteur à spectrométrie de masse (MS).
La méthode s'applique au mesurage des COV non polaires et légèrement polaires à des concentrations allant
de quelques nanogrammes par mètre cube à plusieurs milligrammes par mètre cube. À l'aide des principes
spécifiés dans la présente méthode, certains composés très volatils (COTV) et semi-volatils (COSV) peuvent
également être analysés (voir l'Annexe D).
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 16000-1, Air intérieur — Partie 1: Aspects généraux de la stratégie d'échantillonnage
ISO 16017-1:2000, 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
1) Tenax TA est l'appellation commerciale d'un produit fourni par Buchem. Cette information est donnée à l'intention
des utilisateurs du présent document et ne signifie nullement que l'ISO approuve ou recommande l'emploi exclusif du
produit ainsi désigné. Des produits équivalents peuvent être utilisés s'il est démontré qu'ils conduisent aux mêmes
résultats.
© ISO 2011 – Tous droits réservés 1
---------------------- Page: 7 ----------------------
ISO 16000-6:2011(F)
3 Termes et définitions
Pour les besoins du présent document, les termes et définitions suivants s'appliquent.
3.1
composé organique semi-volatil
COSV
composé organique dont le point d'ébullition se situe entre (240 °C à 260 °C) et (380 °C à 400 °C)
[14]
NOTE 1 Cette classification a été définie par l'Organisation mondiale de la santé .
NOTE 2 Les points d'ébullition de certains composés sont difficiles, voire impossibles à déterminer puisque leur
décomposition intervient avant l'ébullition à pression atmosphérique. La tension de vapeur constitue un autre critère de
classification de la volatilité des composés pouvant servir dans le cadre de la classification de produits chimiques
[15]
organiques .
3.2
composé organique volatil
COV
composé organique dont le point d'ébullition se situe entre (50 °C à 100 °C) et (240 °C à 260 °C)
[14]
NOTE 1 Cette classification a été définie par l'Organisation mondiale de la santé .
NOTE 2 Les points d'ébullition de certains composés sont difficiles, voire impossibles à déterminer puisque leur
décomposition intervient avant l'ébullition à pression atmosphérique. La tension de vapeur constitue un autre critère de
classification de la volatilité des composés pouvant servir dans le cadre de la classification de produits chimiques
[15]
organiques .
3.3
composé organique très volatil
COTV
composé organique dont le point d'ébullition se situe entre <0 °C et (50 °C à 100 °C)
[14]
NOTE 1 Cette classification a été définie par l'Organisation mondiale de la santé .
NOTE 2 Les points d'ébullition de certains composés sont difficiles, voire impossibles à déterminer puisque leur
décomposition intervient avant l'ébullition à pression atmosphérique. La tension de vapeur constitue un autre critère de
classification de la volatilité des composés pouvant servir dans le cadre de la classification de produits chimiques
[15]
organiques .
3.4
composés organiques volatils totaux
COVT
®
somme des composés organiques volatils, échantillonnés sur une cartouche de Tenax TA dont l'élution se
produit entre le n-hexane et le n-hexadécane inclus sur une colonne capillaire non polaire, détectée par
ionisation de flamme (COVT-FID) ou par spectrométrie de masse (COVT-MS) et quantifiée par la conversion
de la surface totale du chromatogramme dans cette fenêtre analytique en équivalent toluène
NOTE Alors que la présente partie de l'ISO 16000 spécifie le dosage de chaque COV, la pratique courante consiste
à générer une valeur de concentration unique afin de caractériser la quantité totale de COV présents dans l'air. Cette
valeur est appelée valeur COVT (voir 11.3 et l'Article 13). Il convient d'insister sur le fait que la valeur COVT ainsi obtenue
dépend des méthodes d'échantillonnage et d'analyse utilisées et qu'il convient par conséquent de l'interpréter en tenant
compte de la description complète de ces méthodes.
4 Principe
Un volume mesuré d'échantillon d'air est recueilli dans une pièce ou dans une chambre d'essai d'émission
(voir l'ISO 16000-9) ou une cellule d'essai d'émission (voir l'ISO 16000-10) à l'aide d'un ou plusieurs tube(s) à
®
sorbant contenant du sorbant Tenax TA . Les composés organiques volatils (COV) sont retenus par le tube à
sorbant et sont analysés par la suite en laboratoire. Les COV recueillis sont désorbés par la chaleur et
2 © ISO 2011 – Tous droits réservés
---------------------- Page: 8 ----------------------
ISO 16000-6:2011(F)
transférés par le gaz vecteur inerte via un piège froid ou un piège à sorbant dans un chromatographe en
phase gazeuse équipé d'une ou plusieurs colonne(s) capillaire(s) et d'un détecteur à ionisation de flamme
et/ou d'un détecteur à spectrométrie de masse.
5 Réactifs et matériaux
5.1 Composés organiques volatils pour étalonnage, de qualité chromatographique.
5.2 Solvant de dilution, pour préparer la solution de mélange d'étalonnage pour dopage de liquide, de
qualité chromatographique, exempt de composés co-éluant avec le(s) composé(s) à l'étude (5.1).
NOTE Dans la plupart des cas, il est avantageux d'utiliser un solvant de dilution considérablement plus volatil que les
COV à analyser. Le méthanol répond communément à ce critère. Les données d'hygiène et de sécurité relatives aux
[24]
composés organiques figurent notamment dans les Fiches internationales de sécurité chimique (ICSC) .
®
5.3 Tenax TA , granulométrie de 0,18 mm à 0,60 mm (30 mesh à 80 mesh).
® ®
Le Tenax TA est un polymère poreux à base d'oxyde de 2,6-diphénylène. Le Tenax TA fabriqué contient de
nombreuses impuretés qui doivent être éliminées avant son utilisation à des fins d'échantillonnage des COV.
®
Procéder au nettoyage du Tenax TA par conditionnement thermique, sous un flux de gaz vecteur pur. Définir
les conditions de nettoyage afin d'éviter toute dégradation du polymère, par exemple à une température de
300 °C pendant 10 h, en utilisant un flux de gaz vecteur à un débit de 50 ml/min à 100 ml/min pour les tubes
®
de prélèvement remplis. Remplir de Tenax TA préalablement nettoyé les tubes de prélèvement
hermétiquement scellés, puis les stocker dans un conteneur fermé, exempt d'émission. Analyser le sorbant
nettoyé afin de confirmer le succès du mode opératoire de nettoyage.
NOTE Des tubes de sorbant pré-remplis, conditionnés (nettoyés) et fermés sont disponibles dans le commerce.
5.4 Atmosphères normalisées, de concentrations connues en un (des) composé(s) à l'étude, préparées
[1]
selon un mode opératoire reconnu. Les méthodes spécifiées dans l'ISO 6141 et dans la partie appropriée
[2]
de l'ISO 6145 conviennent.
3
Préparer des atmosphères normalisées qui équivalent à 100 µg/m environ. Si le mode opératoire n'est pas
appliqué dans des conditions permettant la parfaite traçabilité des concentrations générées en étalons
primaires de masse et/ou de volume ou si l'inertie chimique du système de génération ne peut être garantie,
les concentrations doivent être confirmées à l'aide d'un mode opératoire indépendant.
5.5 Tubes à sorbant normalisés, chargés par dopage dans des atmosphères normalisées (5.4), préparés
en transférant un volume précis d'atmosphère normalisée dans le tube à sorbant, par exemple au moyen
d'une pompe.
Le volume d'échantillon d'atmosphère ne doit pas dépasser le volume de perçage du mélange d'analyte et de
sorbant. Après le chargement, détacher le tube et le refermer. Préparer de nouveaux étalons à chaque lot
d'échantillons. Dans le cadre des essais avec de l'air intérieur et de l'air de chambre d'essai, charger les tubes
à sorbant avec, par exemple, 100 ml, 200 ml, 400 ml, 1 l, 2 l, 4 l ou 10 l de l'atmosphère normalisée
3
sélectionnée à 100 µg/m .
5.6 Solutions de mélange d'étalonnage pour dopage de liquide.
5.6.1 Généralités. La stabilité et les durées de conservation en lieu sûr des solutions de mélange
d'étalonnage doivent être déterminées. De nouvelles solutions normalisées doivent être préparées en fonction
du mode opératoire ou dans le cas de dégradations, dues par exemple à des réactions entre alcools et
cétones. Les concentrations en solution d'étalonnage appropriées varient en fonction des niveaux d'analyte
cible attendus dans chaque lot d'échantillon. Des exemples de préparation de solutions pour une gamme
d'applications sont donnés en 5.6.2 à 5.6.6.
5.6.2 Solution contenant environ 10 mg/ml de chaque composant liquide. Introduire 50 ml de solvant
de dilution dans une fiole jaugée de 100 ml. Peser avec exactitude environ 1 g d'une ou plusieurs
© ISO 2011 – Tous droits réservés 3
---------------------- Page: 9 ----------------------
ISO 16000-6:2011(F)
substance(s) à l'étude dans une fiole jaugée de 100 ml, en commençant par la substance la moins volatile.
Compléter à 100 ml avec du solvant de dilution, boucher et agiter pour homogénéiser.
5.6.3 Solution contenant environ 1 000 µg/ml de chaque composant liquide. Introduire 50 ml de
solvant de dilution dans une fiole jaugée de 100 ml. Ajouter 10 ml de la solution préparée en 5.6.2. Compléter
à 100 ml avec du solvant de dilution, boucher et agiter pour homogénéiser.
5.6.4 Solution contenant environ 100 µg/ml de chaque composant liquide. Introduire 50 ml de solvant
de dilution dans une fiole jaugée de 100 ml. Ajouter 10 ml de la solution préparée en 5.6.3. Compléter à
100 ml avec du solvant de dilution, boucher et agiter pour homogénéiser.
5.6.5 Solution contenant environ 10 µg/ml de chaque composant liquide. Introduire 50 ml de solvant
de dilution dans une fiole jaugée de 100 ml. Ajouter 10 ml de la solution préparée en 5.6.4. Compléter à
100 ml avec du solvant de dilution, boucher et agiter pour homogénéiser.
5.6.6 Solution contenant environ 1 µg/ml de chaque composant liquide. Introduire 50 ml de solvant de
dilution dans une fiole jaugée de 100 ml. Ajouter 10 ml de la solution préparée en 5.6.5. Compléter à 100 ml
avec du solvant de dilution, boucher et agiter pour homogénéiser.
5.7 Tubes à sorbant normalisés, chargés par dopage, préparés en injectant des aliquotes de solutions
normalisées dans des tubes à sorbant propres.
L'extrémité de prélèvement d'un tube à sorbant est ajustée sur le dispositif d'injection du chromatographe en
phase gazeuse (GC) (6.10) balayé par du gaz de purge inerte à un débit de 100 ml/min et une aliquote de 1 µl
à 5 µl d'une solution normalisée appropriée est injectée au travers du septum. Au bout de 5 min, le tube est
détaché, puis refermé. Préparer de nouveaux tubes normalisés à chaque lot d'échantillons.
L'introduction d'étalons liquides dans des tubes à sorbant à l'aide d'un injecteur de chromatographe en phase
gazeuse est considérée comme constituant l'approche optimale en matière d'introduction d'étalons liquides,
car les composés atteignent la couche de sorbant en phase vapeur. Une autre méthode consiste à introduire
des étalons liquides directement dans la couche de sorbant à l'aide d'une seringue (6.3).
Il convient de préparer les mélanges d'étalonnage dans des conditions de température ambiante contrôlée.
Avant utilisation, amener les solutions à l'équilibre de température.
NOTE 1 Lors de la préparation des tubes normalisés contenant des analytes COSV, un transfert efficace est renforcé
si la configuration de l'injecteur permet à la pointe de la seringue d'entrer doucement en contact avec le mécanisme
retenant le sorbant (par exemple grille ou fritté) dans le tube.
NOTE 2 Les tubes normalisés contenant des COTV sont plus généralement préparés à partir d'atmosphères
normalisées (voir 5.4 et 5.5) ou à partir d'étalons gazeux concentrés achetés dans le commerce. La manière appropriée
pour introduire des étalons gazeux concentrés par l'extrémité de prélèvement des tubes de sorbant consiste à utiliser un
courant de gaz vecteur via un injecteur GC non chauffé.
NOTE 3 Si des tubes normalisés sont préparés par introduction d'aliquotes de plus d'une solution étalon ou de plus
d'un gaz étalon, il est approprié d'introduire d'abord l'étalon contenant les composants de plus hauts points d'ébullition et
d'introduire les composants les plus légers en dernier. Cela réduit le risque de perçage de l'analyte durant le processus de
chargement du tube normalisé.
5.8 Tubes normalisés préchargés, disponibles dans le commerce, certifiés, pouvant servir dans le
cadre du contrôle de la qualité analytique et de l'étalonnage de routine.
5.9 Gaz vecteur inerte, par exemple He, Ar, N . Il convient que la pureté du gaz vecteur permette de
2
détecter une injection de 0,5 ng de toluène.
ATTENTION — La qualité du gaz vecteur est de première importance, car les éléments polluants
susceptibles d'être contenus dans les gaz sont enrichis dans le piège froid avec les substances à
analyser.
4 © ISO 2011 – Tous droits réservés
---------------------- Page: 10 ----------------------
ISO 16000-6:2011(F)
6 Appareillage
Appareillage courant de laboratoire et, en particulier, ce qui suit.
6.1 Tubes à sorbant, en acier inoxydable ou en verre, contenant au moins 200 mg de sorbant
®
Tenax TA (5.3), équipés de bouchons à vis en métal et bagues en polytétrafluoroéthylène (PTFE).
Les tubes d'un diamètre externe de 6,4 mm (0,25 pouce), d'un diamètre interne de 5 mm et d'une longueur de
89 mm (3,5 pouces) sont en conformité avec les exigences et sont utilisés dans de nombreux désorbeurs
thermiques disponibles dans le commerce. Utiliser de la laine de verre désactivée ou un autre mécanisme
adapté, par exemple un fritté en acier inoxydable, pour retenir le sorbant dans le tube.
NOTE 1 L'unité de pouce n'est pas autorisée dans les documents ISO; les équivalents en pouce sont donnés
uniquement à titre d'information.
®
Des tubes à sorbant préalablement nettoyés contenant du Tenax TA sont disponibles dans le commerce.
Sinon, des tubes à sorbant peuvent être remplis en laboratoire en procédant comme suit.
Peser la quantité appropriée de sorbant, en utilisant au moins 200 mg de sorbant par tube afin de maintenir la
capacité de sorption. Pour remplir le tube, placer un bouchon de laine de verre désactivée ou une grille en
acier inoxydable dans l'une des extrémités du tube. Transférer le sorbant dans le tube, par aspiration si
nécessaire. Une fois le sorbant versé, placer un bouchon ou une grille supplémentaire afin de retenir le
sorbant dans le tube.
NOTE 2 La détermination du volume de perçage est spécifiée dans l'ISO 16017-1:2000, Annexe B. Les volumes de
perçage s
...
SLOVENSKI STANDARD
oSIST ISO/FDIS 16000-6:2011
01-december-2011
1RWUDQML]UDNGHO 'RORþHYDQMHKODSQLKRUJDQVNLKVSRMLQYQRWUDQMHP]UDNXLQ
]UDNXYSUHVNXVQLKNRPRUDK]DNWLYQLPY]RUþHQMHPQDVRUEHQWX7HQD[7$
WHUPLþQRGHVRUSFLMRLQSOLQVNRNURPDWRJUDILMR]06DOL06),'
Indoor air - Part 6: Determination of volatile organic compounds in indoor and test
chamber air by active sampling on Tenax TA sorbent, thermal desorption and gas
chromatography using MS or MS-FID
Air intérieur -- Partie 6: Dosage des composés organiques volatils dans l'air intérieur des
locaux et chambres d'essai par échantillonnage actif sur le sorbant Tenax TA, désorption
thermique et chromatographie en phase gazeuse utilisant MS ou MS-FID
Ta slovenski standard je istoveten z: ISO 16000-6
ICS:
13.040.20 Kakovost okoljskega zraka Ambient atmospheres
oSIST ISO/FDIS 16000-6:2011 en,fr
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
oSIST ISO/FDIS 16000-6:2011
---------------------- Page: 2 ----------------------
oSIST ISO/FDIS 16000-6:2011
FINAL
INTERNATIONAL ISO/FDIS
DRAFT
STANDARD 16000-6
ISO/TC 146/SC 6
Indoor air —
Secretariat: DIN
Part 6:
Voting begins on:
2011-09-09
Determination of volatile organic
compounds in indoor and test chamber
Voting terminates on:
2011-11-09
air by active sampling on Tenax TA
sorbent, thermal desorption and gas
chromatography using MS or MS-FID
Air intérieur —
Partie 6: Dosage des composés organiques volatils dans l'air intérieur
des locaux et chambres d'essai par échantillonnage actif sur le sorbant
Tenax TA , désorption thermique et chromatographie en phase
gazeuse utilisant MS ou MS-FID
RECIPIENTS OF THIS DRAFT ARE INVITED TO
SUBMIT, WITH THEIR COMMENTS, NOTIFICATION
OF ANY RELEVANT PATENT RIGHTS OF WHICH
THEY ARE AWARE AND TO PROVIDE SUPPORT-
ING DOCUMENTATION.
IN ADDITION TO THEIR EVALUATION AS
Reference number
BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO-
ISO/FDIS 16000-6:2011(E)
LOGICAL, COMMERCIAL AND USER PURPOSES,
DRAFT INTERNATIONAL STANDARDS MAY ON
OCCASION HAVE TO BE CONSIDERED IN THE
LIGHT OF THEIR POTENTIAL TO BECOME STAN-
DARDS TO WHICH REFERENCE MAY BE MADE IN
©
ISO 2011
NATIONAL REGULATIONS.
---------------------- Page: 3 ----------------------
oSIST ISO/FDIS 16000-6:2011
ISO/FDIS 16000-6:2011(E)
Copyright notice
This ISO document is a Draft International Standard and is copyright-protected by ISO. Except as permitted
under the applicable laws of the user's country, neither this ISO draft nor any extract from it may be
reproduced, stored in a retrieval system or transmitted in any form or by any means, electronic,
photocopying, recording or otherwise, without prior written permission being secured.
Requests for permission to reproduce should be addressed to either ISO at the address below or ISO's
member body in the country of the requester.
ISO copyright office
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Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Reproduction may be subject to royalty payments or a licensing agreement.
Violators may be prosecuted.
ii © ISO 2011 – All rights reserved
---------------------- Page: 4 ----------------------
oSIST ISO/FDIS 16000-6:2011
ISO/FDIS 16000-6:2011(E)
Contents Page
Foreword . iv
Introduction . vi
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 2
5 Reagents and materials . 2
6 Apparatus . 4
7 Conditioning and storage of sorbent tubes . 6
7.1 Conditioning . 6
7.2 Storage of conditioned sorbent tubes before sampling . 6
8 Sampling . 6
8.1 Indoor air sampling . 6
8.2 Test chamber air sampling . 6
8.3 Sampling volumes . 7
8.4 Storage of loaded samples . 7
8.5 Field blanks . 7
9 Analysis . 7
9.1 General . 7
9.2 Thermal desorption . 8
9.3 Temperature programme . 8
9.4 Analysis of the samples. 8
10 Identification of single VOCs . 8
11 Concentration of analytes in the sampled air . 9
11.1 General . 9
11.2 Volatile organic compounds . 9
11.3 Total volatile organic compounds . 10
11.4 VVOC and SVOC compounds observed outside the TVOC range . 10
12 Performance characteristics . 11
13 Test report . 12
14 Quality control . 12
Annex A (informative) Examples of compounds detected in indoor air and from building products
in test chambers . 13
Annex B (informative) Safe sampling volumes for selected organic vapours sampled on
Tenax TA . 19
Annex C (informative) Storage recovery of solvents on Tenax TA sorbent tubes . 21
Annex D (informative) Determination of very volatile and semi-volatile organic compounds in
conjunction with volatile organic compounds . 23
Bibliography . 28
© ISO 2011 – All rights reserved iii
---------------------- Page: 5 ----------------------
oSIST ISO/FDIS 16000-6:2011
ISO/FDIS 16000-6:2011(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies
(ISO member bodies). The work of preparing International Standards is normally carried out through ISO
technical committees. Each member body interested in a subject for which a technical committee has been
established has the right to be represented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the
International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 16000-6 was prepared by Technical Committee ISO/TC 146, Air quality, Subcommittee SC 6, Indoor air.
This second edition cancels and replaces the first edition (ISO 16000-6:2004), which has been technically
revised.
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)
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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 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
The following parts are under preparation:
Part 21: Detection and enumeration of moulds — Sampling from materials
Part 27: Determination of settled fibrous dust on surfaces by SEM (scanning electron microscopy)
(direct method)
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 constructions on pollutants and other injurious factors — Inspections
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Introduction
ISO 16000-1 establishes 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. Aspects of the determination (sampling and analysis) and the sampling strategy of specific
pollutants or groups of pollutants are specified in the subsequent parts of ISO 16000 (see Foreword).
ISO 16000-5 (dealing with VOC sampling strategy) is a link between ISO 16000-1 (a generic standard
establishing the principles) and this part of ISO 16000, which deals with sampling and analytical
measurements.
[3]–[7]
ISO 16017 (see Clause 2 and Reference [8]) and ISO 12219 also focus on volatile organic compound
(VOC) measurements.
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FINAL DRAFT INTERNATIONAL STANDARD ISO/FDIS 16000-6:2011(E)
Indoor air —
Part 6:
Determination of volatile organic compounds in indoor and test
chamber air by active sampling on Tenax TA sorbent, thermal
desorption and gas chromatography using MS or MS-FID
1 Scope
This part of ISO 16000 specifies a method for determination of volatile organic compounds (VOCs) in indoor
air and in air sampled for the determination of the emission of VOCs from building products or materials and
other products used in indoor environments using test chambers and test cells. The method uses
1) [13]
Tenax TA sorbent with subsequent thermal desorption (TD) and gas chromatographic (GC) analysis
employing a capillary column or columns and a flame ionization detector (FID) and/or a mass spectrometric
(MS) detector.
The method is applicable to the measurement of non-polar and slightly polar VOCs at concentrations ranging
from sub-micrograms per cubic metre to several milligrams per cubic metre. Using the principles specified in
this method, some very volatile compounds (VVOC) and semi-volatile organic compounds (SVOC) can also
be analysed (see Annex D).
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 16000-1, Indoor air — Part 1: General aspects of sampling strategy
ISO 16017-1:2000, Indoor, ambient and workplace air — Sampling and analysis of volatile organic
compounds by sorbent tube/thermal desorption/capillary gas chromatography — Part 1: Pumped sampling
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
semi-volatile organic compound
SVOC
organic compound whose boiling point is in the range from (240 °C to 260 °C) to (380 °C to 400 °C)
[14]
NOTE 1 This classification has been defined by the World Health Organization .
1) Tenax TA is the trade name of a product supplied by Buchem. 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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NOTE 2 Boiling points of some compounds are difficult or impossible to determine because they decompose before
they boil at atmospheric pressure. Vapour pressure is another criterion for classification of compound volatility that may be
[15]
used for classification of organic chemicals .
3.2
volatile organic compound
VOC
organic compound whose boiling point is in the range from (50 °C to 100 °C) to (240 °C to 260 °C)
[14]
NOTE 1 This classification has been defined by the World Health Organization .
NOTE 2 Boiling points of some compounds are difficult or impossible to determine because they decompose before
they boil at atmospheric pressure. Vapour pressure is another criterion for classification of compound volatility that may be
[15]
used for classification of organic chemicals .
3.3
very volatile organic compound
VVOC
organic compound whose boiling point is in the range from 0 °C to (50 °C to 100 °C)
[14]
NOTE 1 This classification has been defined by the World Health Organization .
NOTE 2 Boiling points of some compounds are difficult or impossible to determine because they decompose before
they boil at atmospheric pressure. Vapour pressure is another criterion for classification of compound volatility that may be
[15]
used for classification of organic chemicals .
3.4
total volatile organic compounds
TVOCs
sum of volatile organic compounds, sampled on Tenax TA , which elute between and including n-hexane and
n-hexadecane on a non-polar capillary column, detected with a flame ionization detector (TVOC-FID) or mass
spectrometric detector (TVOC-MS), and quantified by converting the total area of the chromatogram in that
analytical window to a nominal mass using the chromatographic response factor for toluene (toluene
equivalents)
NOTE While this part of ISO 16000 specifies the determination of individual VOCs, it is common in practice to
generate a single concentration value to characterize the total amount of VOCs present in the air. This value is called the
TVOC value (see 11.3 and Clause 13). It should be emphasized that the TVOC value so obtained depends on the
sampling and analytical methods used, and therefore should be interpreted taking into account the full description of these
methods.
4 Principle
A measured volume of sample air is collected from room air, an emission test chamber (see ISO 16000-9) or
an emission test cell (see ISO 16000-10) by drawing through one (or more) sorbent tube containing
Tenax TA sorbent. Volatile organic compounds (VOCs) are retained by the sorbent tube, and the
compounds are subsequently analysed in the laboratory. The collected VOCs are desorbed by heat and
transferred under inert carrier gas via a cold trap or sorbent trap into a gas chromatograph equipped with a
capillary column or columns and a flame ionization detector and/or a mass spectrometric detector.
5 Reagents and materials
5.1 Volatile organic compounds for calibration, of chromatographic quality.
5.2 Dilution solvent, for preparing calibration blend solution for liquid spiking, of chromatographic quality,
free from compounds co-eluting with the compound(s) of interest (5.1).
NOTE It is in most cases beneficial to use dilution solvent that is considerably more volatile than the VOCs to be
analysed. Methanol most commonly fulfils this criterion. Health and safety data for organic compounds are given, for
[24]
example, in International Chemical Safety Cards (ICSCs) .
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5.3 Tenax TA , particle size 0,18 mm to 0,60 mm (30 mesh to 80 mesh).
Tenax TA is a porous polymer based on 2,6-diphenyleneoxide. Manufactured Tenax TA contains quantities
of impurities, which shall be removed before using it for VOC sampling. Perform cleaning by thermal
conditioning the Tenax TA under a flow of pure carrier gas. Select cleaning conditions so that no degradation
of the polymer occurs, e.g. at temperature of 330 °C for at least 18 h using a carrier gas flow rate of
100 ml/min for packed sampling tubes. Pack pre-cleaned Tenax TA into sampling tubes that are tightly
sealed and store in a closed, emission-free container. Check the success of the cleaning procedure by
performing an analysis of the cleaned sorbent.
NOTE Pre-packed, conditioned (cleaned) and capped sorbent tubes are available commercially.
5.4 Standard atmospheres, of known concentrations of the compound(s) of interest, prepared by a
[1] [2]
recognized procedure. Methods specified in ISO 6141 and the appropriate part of ISO 6145 are suitable.
3
Prepare standard atmospheres equivalent to about 100 µg/m . If the procedure is not applied under
conditions that allow the establishment of full traceability of the generated concentrations to primary standards
of mass and/or volume, or if the chemical inertness of the generation system cannot be guaranteed, the
concentrations shall be confirmed using an independent procedure.
5.5 Standard sorbent tubes, loaded by spiking from standard atmospheres (5.4), prepared by passing an
accurately known volume of the standard atmosphere through the sorbent tube, e.g. by means of a pump.
The volume of atmosphere sampled shall not exceed the breakthrough volume of the analyte-sorbent
combination. After loading, disconnect and seal the tube. Prepare fresh standards with each batch of samples.
For indoor air and test chamber air, load sorbent tubes with e.g. 100 ml, 200 ml, 400 ml, 1 l, 2 l, 4 l or 10 l of
3
the 100 µg/m standard atmosphere selected.
5.6 Calibration blend solutions for liquid spiking.
5.6.1 General. The stability and safe storage times of calibration blend solutions shall be determined. Fresh
standard solutions shall be prepared accordingly or if there is evidence of deterioration, e.g. reactions
between alcohols and ketones. Appropriate calibration solution concentrations vary depending upon expected
target analyte levels in each batch of samples. Examples of solution preparation for a range of applications
are given in 5.6.2 to 5.6.6.
5.6.2 Solution containing approximately 10 mg/ml of each liquid component. Introduce 50 ml of
dilution solvent into a 100 ml volumetric flask. Accurately weigh approximately 1 g of substance or substances
of interest into a 100 ml volumetric flask, starting with the least volatile substance. Make up to 100 ml with
dilution solvent, stopper and shake to mix.
5.6.3 Solution containing approximately 1 000 µg/ml of each liquid component. Introduce 50 ml of
dilution solvent into a 100 ml volumetric flask. Add 10 ml of solution 5.6.2. Make up to 100 ml with dilution
solvent, stopper and shake to mix.
5.6.4 Solution containing approximately 100 µg/ml of each liquid component. Introduce 50 ml of
dilution solvent into a 100 ml volumetric flask. Add 10 ml of solution 5.6.3. Make up to 100 ml with dilution
solvent, stopper and shake to mix.
5.6.5 Solution containing approximately 10 µg/ml of each liquid component. Introduce 50 ml of dilution
solvent into a 100 ml volumetric flask. Add 10 ml of solution 5.6.4. Make up to 100 ml with dilution solvent,
stopper and shake to mix.
5.6.6 Solution containing approximately 1 µg/ml of each liquid component. Introduce 50 ml of dilution
solvent into a 100 ml volumetric flask. Add 10 ml of solution 5.6.5. Make up to 100 ml with dilution solvent,
stopper and shake to mix.
5.7 Standard sorbent tubes, loaded by spiking, prepared by injecting aliquots of standard solutions on to
clean sorbent tubes.
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The sampling end of a sorbent tube is fitted to the unheated injection unit of the gas chromatograph (GC)
(6.10) through which inert purge gas is passed at 100 ml/min, and a 1 µl to 5 µl aliquot of an appropriate
standard solution is injected through the septum. After 5 min, the tube is disconnected and sealed. Prepare
fresh standard tubes with each batch of samples.
Introducing liquid standards on to sorbent tubes via a GC injector is considered the optimum approach to
liquid standard introduction, as components reach the sorbent bed in the vapour phase. Alternatively, liquid
standards may be introduced directly on to the sorbent bed using a syringe (6.3).
Calibration mixtures should be prepared in controlled environmental temperature conditions. Before use,
temper the solutions accordingly.
NOTE 1 When preparing standard tubes containing SVOC analytes, efficient transfer is enhanced if the configuration
of injector allows the tip of the syringe to make gentle contact with the sorbent retaining mechanism (e.g. gauze or frit)
within the tube.
NOTE 2 Standard tubes containing VVOCs are more typically prepared either from standard atmospheres (see 5.4 and
5.5) or from concentrated gas standards sourced commercially. It is appropriate for concentrated gas standards to be
introduced to the sampling end of sorbent tubes in a stream of carrier gas via an unheated GC injector.
NOTE 3 If standard tubes are being prepared by introducing aliquots from more than one standard solution or gas, it is
appropriate first to introduce the standard containing higher boiling components and to introduce the lightest components
last. This minimizes risk of analyte breakthrough during the standard tube loading process.
5.8 Commercial, preloaded standard tubes, certified, are available and can be used for establishing
analytical quality control and for routine calibration.
5.9 Inert carrier gas, e.g. He, Ar, N . The purity of the carrier gas should permit the detection of an
2
injection of 0,5 ng of toluene.
CAUTION — The quality of the carrier gas is of great importance, as contaminants possibly contained
in the gases are enriched in the cold trap together with the substances to be analysed.
6 Apparatus
Ordinary laboratory apparatus and in particular the following.
6.1 Sorbent tubes, of stainless steel or glass, containing at least 200 mg of Tenax TA sorbent (5.3),
with metal screw caps and polytetrafluoroethene (PTFE) ferrules.
Tubes with outside diameter of 6,4 mm (0,25 inch), inside diameter of 5 mm, and of length 89 mm (3,5 inch)
fulfil the requirement and are used in many commercial thermal desorbers. Use deactivated glass wool or
other suitable mechanism, e.g. stainless steel frit, to retain the sorbent in the tube.
NOTE 1 The unit inch is not allowed in ISO documents; inch equivalents are given for information only.
Pre-cleaned sorbent tubes containing Tenax TA are available commercially. Alternatively, sorbent tubes can
be filled in the laboratory as follows.
Weigh the appropriate amount of adsorbent, using no less than 200 mg of sorbent per tube to maintain the
sorption capacity. To pack the tube, insert a plug of deactivated glass wool or a stainless steel gauze into one
end of the tube. Transfer the adsorbent into the tube, assisted by suction if desired. Place an additional plug
or gauze after the sorbent to retain it in the tube.
NOTE 2 The determination of breakthrough volume is specified in ISO 16017-1:2000, Annex B. Breakthrough volumes
are proportional to the dimensions of the sampling tube and quantity of sorbent. As an approximate measure, doubling the
bed length while tube diameter is kept constant doubles the safe sampling volume (SSV).
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6.2 Sorbent tube unions. For sampling, two sorbent tubes connected in series using metal screw-cap
couplings with PTFE ferrules.
6.3 Precision syringes, readable to at least 0,1 µl.
[11] [10]
6.4 Sampling pump, fulfilling the requirements of EN 1232 or ASTM D3686 .
6.5 Tubing, of polyethylene (PE) or PTFE, of appropriate diameter, used to ensure a leak-proof fit to both
pump and sample tube.
Sampling tubes shall not be use
...
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