SIST-TS CEN/TS 13649:2015
(Main)Stationary source emissions - Determination of the mass concentration of individual gaseous organic compounds - Sorptive sampling method followed by solvent extraction or thermal desorption
Stationary source emissions - Determination of the mass concentration of individual gaseous organic compounds - Sorptive sampling method followed by solvent extraction or thermal desorption
This European Standard specifies procedures for the sampling, preparation and analysis of individual volatile organic compounds (VOCs) in waste gas, such as those arising from solvent using processes. It is a reference method.
The results obtained using this Standard are expressed as the mass concentration (mg/m³) of the individual gaseous organic compounds. This Standard is suitable for measuring individual VOCs ranging in concentration from about 0,5 mg/m³ (solid adsorbent / solvent extraction methods) or from about 0,005 mg/m3 (thermal desorption methods). The upper range is defined by the method selected
An Alternative Method may be used provided that the user can demonstrate equivalence to this method according to the Technical Specification CEN/TS 14793, to the satisfaction of his national accreditation body or law.
This standard may be used to meet the monitoring requirements of applicable EC Directives.
This standard may be used for other organic compounds where validated.
This standard is not suitable for measuring total organic carbon (TOC). For the measurement of the mass concentration of total organic carbon then EN 12619 is applicable.
Emissionen aus stationären Quellen - Bestimmung der Massenkonzentration von gasförmigen organischen Einzelverbindungen - Sorptive Probennahme mit Lösemittelextraktion oder thermischer Desorption
Diese Technische Spezifikation legt die Durchführung der Probenahme von einzelnen flüchtigen organischen Verbindungen (VOCs) aus Abgasen, sowie die Aufbereitung und Analyse der Proben fest. Quelle der Abgase können z. B. Prozesse sein, bei denen Lösemittel eingesetzt werden.
Beispiele von einzelnen VOC werden in den relevanten branchenspezifischen BAT-Referenzdokumenten (BREFs) genannt. Die in diesem Dokument beschriebenen Verfahren sind auf gaschromatographisch bestimmbare Verbindungen beschränkt.
Die Messergebnisse werden als Massenkonzentration (mg/m3) der gasförmigen organischen Einzelverbindungen angegeben. Die Messbereiche der VOCs, für die dieses Dokument anwendbar ist, variieren je nach Verbindung und Messverfahren (siehe Anhänge B und C).
Diese Technische Spezifikation kann angewendet werden, um die Anforderungen der Richtlinie über Industrieemissionen (IED) und zugehöriger Dokumente zu erfüllen.
Diese Technische Spezifikation ist nicht für die Messung des gesamten organisch gebundenen Kohlenstoffs (TOC) geeignet. Hierfür ist EN 12619 anzuwenden.
Emissions de sources fixes - Détermination de la concentration massique en composés organiques gazeux individuels - Echantillonnage par adsorption et désorption des solvants ou désorption thermique
La présente Norme européenne spécifie des modes opératoires pour l'échantillonnage, la préparation et l'analyse de composés organiques volatils individuels (COV) dans les effluents gazeux, tels que ceux issus des procédés utilisant des solvants. Elle constitue une méthode de référence.
Les résultats obtenus en utilisant la présente norme sont exprimés en concentration massique (mg/m3) de composés organiques gazeux individuels. La présente norme convient au mesurage des COV individuels dont la concentration avoisine les 0,5 mg/m3 (méthodes par adsorption sur/extraction par solvant) ou les 0,005 mg/m3 (méthodes de thermodésorption). La gamme supérieure varie selon la méthode sélectionnée.
Une autre méthode peut être utilisée à condition que l'utilisateur puisse démontrer l'équivalence de cette méthode, conformément à la Spécification technique CEN/TS 14793, à la satisfaction de l'organisme d'accréditation national ou de la loi en vigueur.
La présente norme peut être utilisée pour répondre aux exigences de surveillance des Directives CE applicables.
La présente norme peut être utilisée pour d'autres composés organiques, sous réserve de validation.
La présente norme ne convient pas au mesurage du carbone organique total (COT). Pour le mesurage de la concentration massique du carbone organique total, l'EN 12619 est applicable.
Emisije nepremičnih virov - Določevanje masne koncentracije posameznih organskih spojin v plinasti fazi - Vzorčenje z adsorpcijo in ekstrakcija s topilom ali termična desorpcija
Ta evropski standard določa postopke za vzorčenje, pripravo in analizo posameznih hlapnih organskih spojin (VOC) v odpadnem plinu, kot so spojine, ki nastanejo pri postopkih, pri katerih se uporablja topilo. To je referenčna metoda.
Rezultati, pridobljeni z uporabo tega standarda, so izraženi kot masna koncentracija (mg/m³) posameznih organskih spojin v plinasti fazi. Ta standard je primeren za merjenje posameznih hlapnih organskih spojin v koncentraciji od približno 0,5 mg/m³ (ekstrakcija z adsorbentom v trdni fazi/ekstrakcija s topilom) ali 0,005 mg/m3 (termična desorpcija). Zgornja meja se določi z izbrano metodo.
Alternativna metoda se lahko uporabi, če lahko uporabnik dokaže njeno enakovrednost s to metodo v skladu s tehnično specifikacijo CEN/TS 14793, ki jo priznava tudi nacionalni akreditacijski organ ali zakonodaja.
Ta standard se lahko uporablja za izpolnitev zahtev glede nadzora iz veljavnih direktiv ES.
Ta standard se lahko uporablja za druge organske spojine, kadar je to potrjeno.
Ta standard ni primeren za merjenje skupnega organskega ogljika (TOC). Za merjenje masne koncentracije skupnega organskega ogljika se uporablja standard EN 12619.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST-TS CEN/TS 13649:2015
01-februar-2015
1DGRPHãþD
SIST EN 13649:2002
(PLVLMHQHSUHPLþQLKYLURY'RORþHYDQMHPDVQHNRQFHQWUDFLMHSRVDPH]QLK
RUJDQVNLKVSRMLQYSOLQDVWLID]L9]RUþHQMH]DGVRUSFLMRLQHNVWUDNFLMDVWRSLORPDOL
WHUPLþQDGHVRUSFLMD
Stationary source emissions - Determination of the mass concentration of individual
gaseous organic compounds - Sorptive sampling method followed by solvent extraction
or thermal desorption
Emissionen aus stationären Quellen - Bestimmung der Massenkonzentration von
gasförmigen organischen Einzelverbindungen - Sorptive Probennahme mit
Lösemittelextraktion oder thermischer Desorption
Emissions de sources fixes - Détermination de la concentration massique en composés
organiques gazeux individuels - Echantillonnage par adsorption et désorption des
solvants ou désorption thermique
Ta slovenski standard je istoveten z: CEN/TS 13649:2014
ICS:
13.040.40 (PLVLMHQHSUHPLþQLKYLURY Stationary source emissions
SIST-TS CEN/TS 13649:2015 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST-TS CEN/TS 13649:2015
TECHNICAL SPECIFICATION
CEN/TS 13649
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
December 2014
ICS 13.040.40 Supersedes EN 13649:2001
English Version
Stationary source emissions - Determination of the mass
concentration of individual gaseous organic compounds -
Sorptive sampling method followed by solvent extraction or
thermal desorption
Emissions de sources fixes - Détermination de la Emissionen aus stationären Quellen - Bestimmung der
concentration massique en composés organiques gazeux Massenkonzentration von gasförmigen organischen
individuels - Échantillonnage par adsorption et extraction Einzelverbindungen - Sorptive Probenahme und
par solvant ou thermodésorption Lösemittelextraktion oder thermische Desorption
This Technical Specification (CEN/TS) was approved by CEN on 25 August 2014 for provisional application.
The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to submit their
comments, particularly on the question whether the CEN/TS can be converted into a European Standard.
CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS available
promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the CEN/TS)
until the final decision about the possible conversion of the CEN/TS into an EN is reached.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United
Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2014 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 13649:2014 E
worldwide for CEN national Members.
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Contents Page
Foreword .4
1 Scope .5
2 Normative references .5
3 Terms and definitions .5
4 Principle .6
5 Apparatus and materials .6
5.1 Method of measurement .6
5.2 Sampling system .8
5.3 Sampling tubes .8
5.3.1 Sampling tubes for solvent extraction .8
5.3.2 Sampling tubes for thermal desorption.8
5.4 Pumps and other devices for sampling .8
5.5 Gas volume meter .9
5.6 Analytical reagents .9
5.6.1 General .9
5.6.2 Extraction solvent (for solvent extraction) .9
5.6.3 Reference materials for calibration of the analytical procedure .9
5.7 Analytical apparatus . 10
5.7.1 Capillary gas chromatograph (GC) . 10
5.7.2 Thermal desorber (for thermal desorption) . 10
6 Sampling procedure . 10
6.1 General . 10
6.2 Sampling conditions . 10
6.3 Measurement of waste gas sample volume . 11
6.4 Control of leakage. 11
6.5 Handling, storage, transport of sampled tubes . 11
6.5.1 General . 11
6.5.2 Activated carbon (charcoal) tubes . 11
6.5.3 Thermal desorption tubes . 12
6.6 Blanks . 12
6.6.1 Field blanks . 12
6.6.2 Analytical (laboratory) blanks . 12
6.6.3 Solvent blank . 12
7 Analytical procedure . 12
7.1 Calibration of the GC analysis . 12
7.1.1 GC calibration for analysis of solvent extracts . 12
7.1.2 Calibration for thermal desorption analysis . 13
7.2 Sample preparation (desorption/extraction) . 13
7.2.1 Solvent desorption . 13
7.2.2 Thermal desorption . 14
7.3 Analysis . 14
7.3.1 GC analysis of extract from activated carbon tubes. 14
7.3.2 Thermal desorption / GC analysis of sorbent tubes . 14
7.4 Quantification of individual organic compound concentrations . 15
8 Calculation of results . 16
8.1 Concentration . 16
8.2 Uncertainty . 16
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9 Quality control . 16
9.1 General . 16
9.2 Performance requirements . 17
9.2.1 Sampling. 17
9.2.2 Analytical . 17
10 Report . 18
Annex A (normative) Sample trains . 19
Annex B (informative) Solvent extraction of activated charcoal tubes . 23
Annex C (informative) Additional information on flue gas sampling using thermal desorption
tubes . 24
Annex D (informative) Validation of monitoring methods for speciated organic substances in
stack gas . 27
Annex E (informative) Safety measures . 45
Bibliography . 46
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Foreword
This document (CEN/TS 13649:2014) has been prepared by Technical Committee CEN/TC 264 “Air quality”,
the secretariat of which is held by DIN.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN 13649:2001.
Significant technical changes between this Technical Specification and the previous edition of EN 13649 are:
a) the status of the document has been changed from European Standard (EN) to Technical Specification
(TS);
b) the scope has been clarified regarding the use of the TS and its applicability;
c) a decision tree for the determination of the sampling procedure has been included;
d) the sampling strategy has been aligned with EN 15259;
e) the thermal desorption technique has been added;
f) comprehensive information on the validation of monitoring methods for speciated organic substances in
stack gas is given.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to announce this Technical Specification: Austria, Belgium, Bulgaria, Croatia, Cyprus,
Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany,
Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,
Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.
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1 Scope
This Technical Specification specifies procedures for the sampling, preparation and analysis of individual
volatile organic compounds (VOCs) in waste gas, such as those arising from solvent using processes.
Sampling occurs by adsorption on sorbents, preparation by solvent extraction or thermodesorption and
analysis by gas chromatography.
Examples of individual VOC are given in relevant industry sector BAT Reference documents (BREFs).
3
The results obtained are expressed as the mass concentration (mg/m ) of the individual gaseous organic
compounds. This document is suitable for measuring individual VOCs whose ranges vary depending on
compound and test method, refer to Annex B and C.
This Technical Specification may be used to meet the monitoring requirements of the Industrial Emission
Directive (IED) and associated supporting documents.
This Technical Specification is not suitable for measuring total organic carbon (TOC). For the measurement of
the mass concentration of total organic carbon then EN 12619 [3] is applicable.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated references,
the latest edition of the referenced document (including any amendments) applies.
EN 15259, Air quality - Measurement of stationary source emissions - Requirements for measurement
sections and sites and for the measurement objective, plan and report
EN ISO 14956, Air quality - Evaluation of the suitability of a measurement procedure by comparison with a
required measurement uncertainty (ISO 14956)
EN ISO 16017-1, Indoor, ambient and workplace air - Sampling and analysis of volatile organic compounds by
sorbent tube/thermal desorption/capillary gas chromatography - Part 1: Pumped sampling (ISO 16017-1)
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
desorption efficiency
ratio of the mass of the recovered organic material to the mass of organic material collected by the adsorbent
expressed as a percentage
3.2
sampling tube for solvent extraction
glass tube filled with activated carbon as the adsorbent
3.3
sampling tubes for thermal desorption
stainless steel, inert-coated steel or glass tube-form samplers supplied capped and packed with one or more
conditioned, thermal desorption compatible sorbents
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3.4
uncertainty
parameter associated with the result of a measurement, that characterizes the dispersion of the values that
could reasonably be attributed to the measurand
[SOURCE: ISO/IEC Guide 98-3:2008 [2]]
3.5
volatile organic compound
VOC
any organic compound having at 293,15 K a vapour pressure of 0,01 kPa or more, or having a corresponding
volatility under the particular conditions of use
3.6
field blank
value determined by a specific procedure used to ensure that no significant contamination has occurred
during all steps of the measurement and to check that the operator can achieve a quantification level adapted
to the task
4 Principle
There are three steps in the measurement of individual gaseous organic compounds: sampling, desorption
and analysis.
Sampling approaches vary depending on waste gas conditions. Suitable sorbent shall be selected. This
document specifies solvent extraction or thermal desorption. Analysis is by gas chromatography.
Other methods may also be applicable e.g. canister, as an alternative to sorbent sampling for very volatile
compounds, or condensate trap (catchpot) sampling systems, as an alternative to dilution sampling, providing
their suitability can be demonstrated, e.g. according to CEN/TS 14793 [1].
Figure 1 shows the decision tree for determining the sampling procedure.
5 Apparatus and materials
5.1 Method of measurement
The sample gas is extracted from the waste gas exhaust duct via a sampling system and onto a solid sorbent
tube using a pump. The solid sorbent tube is then solvent extracted or thermally desorbed and the compounds
are determined by gas chromatography.
Many of the solvent using processes covered by the Industrial Emissions Directive produce waste gases
which do not have a high water content. This document requires the use of a dilution sampling system when
the concentration of water or solvent is high enough to cause the risk of condensation.
3
NOTE The limit values of EU Directives are expressed in mg/m , on a wet basis, for non-combustion process and on
a dry basis, for combustion processes, at the reference conditions of 273 K and 101,3 kPa.
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Figure 1 — Decision tree for determination of sampling procedure
Liquid water interferes with the sorption process and shall not be allowed to reach the sorbent material
(activated carbon or thermal desorption compatible sorbents). There shall be no visible condensation within
the tube.
Drying tubes, e.g. sodium sulfate, shall not be used upstream of the sorbent because of the risk of VOC
losses.
Sorbent sampling methods (activated carbon or thermal desorption-compatible) are only compatible with the
vapour-phase fraction of semi-volatile compounds. Any particulates in the sample gas shall be entrained on
filters before the sample is allowed to reach the sorbent bed.
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5.2 Sampling system
The set-up of a suitable sampling system is shown in Annex A.
The sampling system shall be made of materials which are chemically and physically inert to the constituents
of the gaseous effluent. Glass, PTFE and polypropylene fluoride or any other material for which it has been
shown that they do not absorb or react with compounds present in the sample gas at the temperature
considered, are suitable. To avoid contamination from particulate, a dust filter shall be used. This should be
heated if necessary, depending on application.
5.3 Sampling tubes
5.3.1 Sampling tubes for solvent extraction
The sorbent tube, filled with activated carbon as the adsorbent, shall have the following characteristics:
— a main adsorbent layer containing 100 mg of activated carbon with a glass wool plug at the front of the
tube;
— a security adsorbent layer to detect breakthrough, containing 50 mg of activated carbon separated from
the front layer.
Sorbent tubes shall be used in accordance with the manufacturer’s instructions to avoid leakage and sample
loss. Open or used carbon tubes shall not be reused.
NOTE A suitable type of tubes is NIOSH type B with closed melted ends.
5.3.2 Sampling tubes for thermal desorption
Stainless steel, inert-coated steel or glass samplers supplied capped and packed with one or more
conditioned, thermal desorption compatible sorbents shall be used for organic vapour sampling and
subsequent thermal desorption analysis. See Annex C and EN ISO 16017-1 for more details. The sampling
end of an identical, secondary (back-up) tube can be connected to the outlet of the primary sampling tube as a
check on breakthrough. See 6.3 and Annex C for more information. Unions for connecting the two tubes in
series shall comprise inert materials such as stainless steel, coated stainless steel or PTFE and shall not
damage tube ends.
NOTE Stainless steel (or inert-coated steel) compression couplings fitted with combined PTFE ferrules have been
found to be effective for connecting sample tubes together in series.
Thermal desorption sampling tubes can be re-used many times (typically > 100 thermal cycles).
Conditioned tubes shall be considered sufficiently clean if individual artefact masses do not exceed 10 % of
the mass retained when sampling flue gases at the lowest concentration of interest. See also 6.6.
5.4 Pumps and other devices for sampling
A sampling pump or some alternative means of pulling a controlled flow or volume of waste gas through the
sampling system and onto the sampling tube is required. The pump or alternative flow controlled sampling
system shall have an adjustable flow rate (e.g. up to 0,1 l/min for thermal desorption tubes or up to 0,5 l/min
for charcoal tubes); typical flow rate and sample volume ranges for activated carbon and thermal desorption
tubes are given in Annex B and Annex C respectively.
As thermal desorption typically offers three orders of magnitude more sensitivity than solvent extraction, it also
allows the option of collecting small sample volumes. For example, if individual organic compounds are
3
present above 500 µg/m , a sample volume of 100 ml is usually sufficient for thermal desorption/GC analytical
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sensitivity. Such small aliquots can be accurately drawn onto the sorbent tubes using simple bellows-type
pumps or even by slowly withdrawing the plunger of a large gas syringe.
NOTE Such ‘grab’ sampling methods are only suitable for steady-state emissions. They are not suitable for time
weighted average monitoring of variable waste gas concentrations e.g. when monitoring emissions throughout the
duration of a specific batch process, unless multiple sequential emission samples are collected.
The pump or alternative sampling mechanism shall be placed downstream of the sorbent tube and coupled to
the non-sampling end of the sorbent tube or sorbent tube assembly. See Annex B and Annex C for more
information.
5.5 Gas volume meter
The volume of the gas sampled shall be measured using a calibrated device, e.g. gas volume meter or
calibrated pump, providing the volume is measured with a relative uncertainty not exceeding 5 % at actual
conditions. The uncertainty of the measurement of the temperature and the pressure, shall be less than 2,5 °C
and less than 1,0 % respectively.
5.6 Analytical reagents
5.6.1 General
Only reagents of analytical grade or better quality shall be used unless otherwise stated.
5.6.2 Extraction solvent (for solvent extraction)
Extraction solvents, for solvent extraction, shall be of chromatographic quality and free from compounds co-
eluting with the compounds of interest.
NOTE Carbon disulphide (CS ) is a suitable extraction solvent for most of the compounds likely to be encountered in
2
solvent using processes.
Beware of low and variable recovery rates for polar compounds. Use of additional or alternative extraction
solvents may improve recovery in these cases.
5.6.3 Reference materials for calibration of the analytical procedure
The chromatographic system shall be calibrated with those reference materials which correspond to the
compounds likely to arise in the process under investigation.
For calibrating solvent extraction methods the reference materials shall be prepared in a solution of the
extraction solvent to be used. The extraction solvents are highly volatile and fresh reference standards shall
be prepared regularly.
For calibrating thermal desorption methods, liquid or gas phase standards may be used. See 7.1.2 and
EN ISO 16017-1 for more information.
Liquid standards for thermal desorption should be prepared in a ‘carrier’ solvent that is free from interfering
artefacts. Choose a solvent that can either be selectively purged from tube during the standard loading
process (see 7.1.2) or that can be chromatographically resolved from the compounds of interest during
analysis.
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5.7 Analytical apparatus
5.7.1 Capillary gas chromatograph (GC)
Laboratory apparatus suitable for capillary column gas chromatography shall be used.
5.7.2 Thermal desorber (for thermal desorption)
The thermal desorber is connected to the GC (or GC-MS). It is used for the two stage thermal desorption of
sorbent tubes and transfer of the desorbed vapours via an inert gas flow into a gas chromatograph. A typical
apparatus contains a mechanism for holding the tubes to be desorbed while they are heated and purged
simultaneously with inert carrier gas. The desorption temperature and time is adjustable, as is the carrier gas
flow rate. The apparatus should also incorporate additional features such as leak testing, a cold trap in the
transfer line to concentrate the desorbed sample and at least one, preferably two quantitative sample split
points. The desorbed sample contained in the purge gas, is routed to the gas chromatograph and capillary
column via a heated transfer line.
Optional features to be considered include internal standard addition, automatic dry purging for simplifying the
analysis of humid samples and re-collection of split flow for repeat analysis and validation of compound
recovery (see Annex C).
6 Sampling procedure
6.1 General
The requirements of EN 15259 shall be met.
NOTE The homogeneity tests specified in EN 15259 can be performed using direct read-out FID instruments in
accordance with EN 12619 [3] providing the FID signal obtained is representative of the compound of interest.
6.2 Sampling conditions
The test laboratory shall have a documented procedure, to describe how to determine an appropriate
sampling volume and time. The temperature of the sample gas reaching the sorbent tube shall not be allowed
to exceed 40 °C. The sampling time and volume shall be calculated using
— the estimated concentration and/or limit value,
— the lower limit of detection of the analysis method,
— the safe sampling volume or capacity of the tube for the compounds of interest at the relevant sampling
temperature, i.e. a volume of not more than 70 % of the 5 %-breakthrough volume or 50 % of the
retention volume,
— the process time e.g. batch process time.
NOTE 1 Sample time and duration may be specified by the regulatory authority.
NOTE 2 If information on total VOC concentration in the waste gas is available from FID or some other stack
monitoring device, this can be useful in determining suitable sampling volumes.
Typical sample flow rates and sample volumes for charcoal tubes and thermal desorption are described in
Annex B and Annex C respectively.
In all cases, the volume, duration and frequency of sampling shall be sufficient to ensure that the quantitative
data obtained is representative of the mean compound concentration in the waste gas for the duration of the
process being monitored or over the period of sampling. To ensure representative sampling when collecting
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small volumes of waste gas, the volume of the sampling system shall be taken into account and flushed with
waste gas immediately before the start of sampling.
A continuously flushed sampling system with a ‘Tee-ed’ bypass line can also be used. If compound
breakthrough or sample overload are particular concerns due to high compound volatility or high flue gas
concentrations; sampled volumes should be minimised. In the case of monitoring steady-state emissions with
thermal desorp
...
SLOVENSKI STANDARD
oSIST prEN 13649:2011
01-junij-2011
(PLVLMHQHSUHPLþQLKYLURY'RORþHYDQMHPDVQHNRQFHQWUDFLMHSRVDPH]QLK
RUJDQVNLKVSRMLQYSOLQDVWLID]L0HWRGD]DNWLYQLPRJOMHPLQGHVRUSFLMHVWRSLORP
Stationary source emissions - Determination of the mass concentration of individual
gaseous organic compounds - Active carbon and solvent desorption method
Emissionen aus stationären Quellen - Bestimmung der Massenkonzentration von
einzelnen gasförmigen organischen Verbindungen - Aktivkohleadsorptions- und
Lösemitteldesorptionsverfahren
Emissions de sources fixes - Détermination de la concentration massique en composés
organiques gazeux individuels - Méthode par charbon actif et désorption des solvants
Ta slovenski standard je istoveten z: prEN 13649
ICS:
13.040.40 (PLVLMHQHSUHPLþQLKYLURY Stationary source emissions
oSIST prEN 13649:2011 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN 13649:2011
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oSIST prEN 13649:2011
EUROPEAN STANDARD
DRAFT
prEN 13649 rev
NORME EUROPÉENNE
EUROPÄISCHE NORM
April 2011
ICS 13.030.40 Will supersede EN 13649:2001
English Version
Stationary source emissions - Determination of the mass
concentration of individual gaseous organic compounds - Active
carbon and solvent desorption method
Emissions de sources fixes - Détermination de la Emissionen aus stationären Quellen - Bestimmung der
concentration massique en composés organiques gazeux Massenkonzentration von einzelnen gasförmigen
individuels - Méthode par charbon actif et désorption des organischen Verbindungen - Aktivkohleadsorptions- und
solvants Lösemitteldesorptionsverfahren
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee CEN/TC 264.
If this draft becomes a European Standard, CEN members are bound to comply with the CEN/CENELEC Internal Regulations which
stipulate the conditions for giving this European Standard the status of a national standard without any alteration.
This draft European Standard was established by CEN in three official versions (English, French, German). A version in any other language
made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,
Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
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 supporting documentation.
Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without notice and
shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2011 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 13649 rev:2011: E
worldwide for CEN national Members.
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Contents Page
Foreword .3
1 Scope .3
2 Normative references .3
3 Terms and definitions .4
4 Principle .5
5 Apparatus and materials .5
6 Sampling procedure .9
7 Analytical procedure . 11
8 Calculation of waste gas concentrations . 15
9 Quality control . 15
10 Report . 15
Annex A (normative) Sample trains . 17
Annex B (normative) Additional information on flue gas sampling using thermal desorption tubes . 24
Annex C (normative) Solvent extraction of activated charcoal tubes . 26
Annex D (informative) Safety measures. 27
Annex E (informative) Significant technical changes . 28
Bibliography . 29
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Foreword
This document (prEN 13649:2011) has been prepared by Technical Committee CEN/TC 264 “Air quality”, the
secretariat of which is held by DIN.
This document is currently submitted to the CEN Enquiry.
This document will supersede EN 13649:2011.
This European Standard has been prepared under a mandate given to CEN by the European Commission
and European Free Trade Association.
The Annexes A, B, C are normative, D and E are informative.
1 Scope
This European Standard specifies procedures for the sampling, preparation and analysis of individual volatile
organic compounds (VOCs) in waste gas, such as those arising from solvent using processes. It is a
reference method.
The results obtained using this standard are expressed as the mass concentration (mg/m³) of the individual
gaseous organic compounds. This Standard is suitable for measuring individual VOCs ranging in
concentration from about 0,5 mg/m³ (solid adsorbent/solvent extraction methods) or from about
0,005 mg/m³ (thermal desorption methods). The upper range is defined by the method selected.
An alternative Method may be used provided that the user can demonstrate equivalence to this method
according to the Technical Specification CEN/TS 14793, to the satisfaction of his national accreditation body
or law.
This standard may be used to meet the monitoring requirements of applicable EC Directives.
This standard may be used for other organic compounds where validated.
This standard is not suitable for measuring total organic carbon (TOC). For the measurement of the mass
concentration of total organic carbon then EN 12619 is applicable.
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.
EN15259, Air quality — Measurement of stationary source emissions — Requirements for measurement
sections and sites and for the measurement objective, plan and report
EN14789, Stationary source emissions — Determination of volume concentration of oxygen (O ) —
2
Reference method — Paramagnetism
EN 14790, Stationary source emissions — Determination of the water vapour in ducts
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ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results — Part 1: General
principles and definitions
ISO 9169, Air Quality — Determination of performance characteristics of measurement methods
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
condensate trap
vessel designed to remove moisture from the sample waste gas
3.2
desorption efficiency
ratio of the mass of the recovered organic material to the mass of organic material collected by the
adsorbent expressed as a percentage
3.3
detection limit
minimum concentration of a compound which produces an observable response, as referred to in ISO 9169
3.4
dilution gas
gas used to dilute sampled waste gas to prevent water condensation
3.5
gaseous waste product
gaseous waste product from an industrial-scale process in which solvent or some other potentially toxic or
odorous organic chemical vapour may be present Reference conditions
The limit values of EU Directives are expressed in mg/m³, on a wet basis, for non combustion process and on
a dry bases, for combustion processes, at the reference conditions of 273 K and 101,3 kPa.
3.6
sampling tube for solvent extraction
commercially available glass tube filled with activated carbon or similar as the adsorbent
3.7
sampling tubes for thermal desorption
stainless steel, inert-coated steel or glass samplers supplied capped and packed with one or more
conditioned, thermal desorption compatible sorbents
3.8
uncertainty
parameter associated with the result of a measurement, that characterizes the dispersion of the values that
could reasonably be attributed to the measurand
3.9
uncertainty budgets
calculation table combining all the sources of uncertainty according to ISO 14956 or ENV 13005 in order to
calculate the overall uncertainty of the method at a specified value
3.10
overall uncertainty
expanded combined standard uncertainty attached to the measurement result calculated according to ENV
13005
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3.11
VOC
definition from solvent directive:
Volatile organic compound (VOC) shall mean any organic compound having at 293,15 K a vapour pressure of
0,01 kPa or more, or having a corresponding volatility under the particular conditions of use. For the purpose
of this Directive, the fraction of creosote which exceeds this value of vapour pressure at 293,15 K shall be
considered as a VOC;
4 Principle
There are three steps in the measurement of individual gaseous organic compounds; sampling, capture and
analysis.
Sampling approaches vary depending on waste gas conditions. Suitable capture medium must be selected.
Solvent extraction or thermal desorption may be used. Analysis is by gas chromatography.
5 Apparatus and materials
5.1 Method of measurement
The sample gas is extracted from the waste gas exhaust duct via a sampling system and onto a solid sorbent
tube using a pump. The solid sorbent tube is then solvent extracted or thermally desorbed and the compounds
are determined by gas chromatography.
Many of the solvent using processes covered by the Council Directive 1999/13/EEC produce waste gases
which do not have a high water content. Where high solvent concentrations or the condensation of water
vapour is expected, this European Standard requires the use of dilution or condensate trap sampling system
e.g. catchpot sampling systems (see Annex A). When condensate trap sampling systems are used then the
condensate must be analysed.
Liquid water interferes with the sorption process and shall not be allowed to reach the sorbent material
(activated carbon or thermal desorption compatible sorbents).
Drying tubes, e.g. sodium sulphate, shall not be used because of the risk of VOC losses.
NOTE Sorbent sampling methods (activated carbon or TD-compatible) are only compatible with the vapour-phase
fraction of semi-volatile compounds. Any particulates in the sample gas must be entrained on filters before the sample is
allowed to reach the sorbent bed.
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5.2 Sampling system
Figure 1 — Decision tree for determination of sampling procedure
The set-up of a suitable sampling system, is shown in Annex A.
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All components of the sampling system shall be made of suitable inert material, i.e. must not interfere with the
compound that is being determined. To avoid contamination from particulate a dust filter shall be provided.
Other methods of sampling can be used e.g. dilution or canister sampling, see Annex A.
NOTE Canisters are also predominantly used for ‘grab’ sampling not time weighted average monitoring (see Annex
A).
5.3 Sampling tubes
5.3.1 Sampling tubes for solvent extraction
The sorbent tube, filled with activated carbon as the adsorbent, shall have the following characteristics:
a main adsorbent layer containing not less than 100 mg of activated carbon;
a security adsorbent layer to detect breakthrough, containing not less than 50 mg of activated carbon;
NOTE 1 Suitable types of tubes are NIOSH type B filled 100mg with activated carbon prepared from coconut shell and
50 mg in the security layer. For higher concentration then NIOSH Type G (750 mg main adsorbent layer, 250 mg security
adsorbent layer) can be used.
the sorbent tube construction material shall be inert.
NOTE 2 A suitable material is glass; the fresh tubes are closed by melted ends.
Sampling tubes shall be considered sufficiently clean if individual artefact masses do not exceed 10 % of the
mass retained when sampling flue gases at the lowest concentration of interest e.g. 10 % of emission limit
values
Sorbent tubes shall be used in accordance with the manufacturer’s instructions to avoid leakage and sample
loss. Open or used carbon tubes shall not be reused.
5.3.2 Sampling tubes for thermal desorption
Stainless steel, inert-coated steel or glass samplers supplied capped and packed with one or more
conditioned, thermal desorption compatible sorbents shall be used for organic vapour sampling and
subsequent thermal desorption analysis. See Annex B and EN ISO 16017-1 for more details. The sampling
end of an identical, secondary (back-up) tube can be connected to the outlet of the primary sampling tube as a
check on breakthrough. See 6.3 and Annex B for more information. Unions for connecting the two tubes in
series shall comprise inert materials such as stainless steel, coated stainless steel or PTFE and must not
damage tube ends.
NOTE 1 Stainless steel (or inert coated steel) compression couplings fitted with combined PTFE ferrules have been
found to be effective for connecting sample tubes together in series.
Thermal desorption sampling tubes can be re-used many times (typically > 100 thermal cycles).
NOTE 2 While thermal desorption sampling tubes can be re-used many times and while the process of thermal
desorption inherently re-conditions the tubes during analysis, care must be taken to ensure that artefact levels do not
interfere with measurement.
Conditioned tubes shall be considered sufficiently clean if individual artefact masses do not exceed 10 % of
the mass retained when sampling flue gases at the lowest concentration of interest e.g. 10 % of emission limit
values. See also 6.7.
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5.4 Pumps and other devices for sampling
A sampling pump or some alternative means of pulling a controlled flow or volume of waste gas through the
sampling system and onto the sampling tube is required. The pump or alternative flow controlled sampling
system shall have an adjustable flow rate (e.g. up to 100 ml/min for thermal desorption tubes or up to 1 l/min
for charcoal tubes); typical flow rate and sample volume ranges for activated carbon and thermal desorption
tubes are given in Annexes C and B respectively.
As thermal desorption typically offers three orders of magnitude more sensitivity than solvent extraction, it also
allows the option of collecting small sample volumes. For example; if individual organic compounds are
present above 500 µg/m³, a sample volume of 100 ml is usually sufficient for thermal desorption/GC analytical
sensitivity. Such small aliquots can be accurately drawn onto the sorbent tubes using simple bellows-type
pumps or even by slowly withdrawing the plunger of a large gas syringe.
NOTE Such ‘grab’ sampling methods are only suitable for steady-state emissions. They are not suitable for time
weighted average monitoring of variable waste gas concentrations e.g. when monitoring emissions throughout the
duration of a specific batch process, unless multiple sequential emission samples are collected.
The pump or alternative sampling mechanism shall be placed downstream of the sorbent tube and coupled to
the non-sampling end of the sorbent tube or sorbent tube assembly. See Annexes B and C for more
information.
5.5 Gas volume meter
The volume of the gas sampled shall be measured using a calibrated device, e.g. gas volume meter or
calibrated pump, providing the volume is measured with a relative uncertainty not exceeding ± 5 % at actual
conditions. The uncertainty of the measurement of the temperature and the pressure, if required for reporting
at standard conditions, shall be less than ± 2,5 K and less than ± 1,0 % respectively.
5.6 Analytical reagents
5.6.1 General
Only reagents of recognised analytical grade or better quality shall be used unless otherwise stated.
5.6.2 Extraction solvent (for solvent extraction)
Extraction solvents, for solvent extraction, shall be of chromatographic quality and free from compounds co-
eluting with the compounds of interest.
NOTE 1 Carbon disulphide (CS ) is a suitable extraction solvent for most of the compounds likely to be encountered
2
in solvent using processes.
NOTE 2 Beware of low and variable recovery rates for polar compounds, particularly from humid samples. Use of
additional or alternative extraction solvents may improve recovery in these cases.
5.6.3 Reference materials for calibration of the analytical procedure
The chromatographic system shall be calibrated with those reference materials which correspond to the
compounds likely to arise in the process under investigation.
For calibrating solvent extraction methods the reference materials shall be prepared in a solution of the
extraction solvent to be used. The extraction solvents are highly volatile and fresh reference standards shall
be prepared regularly.
For calibrating thermal desorption methods, liquid or gas phase standards may be used. See 7.1.2 and
EN ISO 16017-1 for more information.
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NOTE Liquid standards for thermal desorption should be prepared in a ‘carrier’ solvent that is free from interfering
artefacts. Choose a solvent that can either be selectively purged from tube during the standard loading process (see
Section 7.1.2) or that can be chromatographically resolved from the compounds of interest during analysis.
In both cases (liquid extraction and thermal desorption), the range between the lowest and highest level
standard shall be at least a factor of 20.
5.7 Analytical apparatus
5.7.1 Capillary gas chromatograph (GC)
Laboratory apparatus suitable for capillary column gas chromatography shall be used.
5.7.2 Thermal desorber (for thermal desorption)
The thermal desorber is connected to the GC (or GC/MS). It is used for the two stage thermal desorption of sorbent
tubes and transfer of the desorbed vapours via an inert gas flow into a gas chromatograph. A typical apparatus
contains a mechanism for holding the tubes to be desorbed whilst they are heated and purged simultaneously
with inert carrier gas. The desorption temperature and time is adjustable, as is the carrier gas flow rate. The
apparatus should also incorporate additional features such as automatic sample tube loading, leak testing, a
cold trap in the transfer line to concentrate the desorbed sample and at least one, preferably two, quantitative
sample split points. The desorbed sample contained in the purge gas, is routed to the gas chromatograph and
capillary column via a heated transfer line.
Optional features to be considered include internal standard addition, automatic dry purging for simplifying the
analysis of humid samples and re-collection of split flow for repeat analysis and validation of compound
recovery (see Annex B).
6 Sampling procedure
6.1 General
The requirements of EN 15259 shall be met.
NOTE The homogeneity tests specified in EN 15259 can be performed using direct read-out FID instruments in
accordance with EN 12619 providing it is representative of the compound of interest.
6.2 Sampling time, volume and flow rate
The test laboratory shall have a documented procedure, to describe how to determine an appropriate
sampling volume and time. The sampling time and volume shall be calculated using the estimated
concentration and/or limit value, the lower limit of detection of the analysis method and the breakthrough
volume or capacity of the tube for the compounds concerned.
NOTE 1 If information on total VOC concentration in the waste gas is available from FID or some other stack
monitoring device, this can be useful in determining suitable sampling volumes.
Typical sample flow rates and sample volumes for thermal desorption and charcoal tubes are described in
Annexes B and C respectively.
In all cases, the volume, duration and frequency of sampling shall be sufficient to ensure that the quantitative
data obtained is representative of the mean compound concentration in the waste gas for the duration of the
process being monitored or over the period of sampling. To ensure representative sampling when collecting
small volumes of waste gas, the volume of the sampling system shall be taken into account and flushed with
waste gas immediately before the start of sampling.
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NOTE 2 A continuously flushed sampling system with a ‘Tee-ed’ bypass line can also be used. If compound
breakthrough or sample overload are particular concerns due to high compound volatility or high flue gas concentrations;
sampled volumes shall be minimised. In the case of monitoring steady-state emissions with thermal desorption tubes
this can be achieved using simple grab-sampling apparatus (see Section 5.4). However, for time weighted average
monitoring and whenever using pumps or similar flow-controlled apparatus, sampling small waste gas volumes may be
subject to higher error – depending on the respective flow rate range of the pump/device selected. In this case, gas
dilution shall be used to maintain sampling flow rates and volumes at an accurate level while minimising risk of sample
overload and breakthrough. Dilution can be either static or dynamic (see Annex B).
Sample overload or breakthrough shall be controlled by separate analysis of the second section (activated
carbon tubes) or secondary back-up tubes (thermal desorption). See 5.3.2 and Annex B for more information.
Maximum breakthrough allowed shall be less than 5 % of the overall concentration (see 9).
NOTE 3 If analytical data obtained from the second layer or secondary (back-up) tube is below the detection limit, it is
accepted that there is no breakthrough.
6.3 Measurement of waste gas sample volume
The volume of the gas sampled shall be determined using a calibrated sampling device, see 5.5. See Annex A
for details of sample train components.
The sample temperature and pressure at the gas meter shall be measured unless automatically compensated
for by the sampling device.
6.4 Control of leakage
Leakage contributes significantly to sampling errors and shall be controlled by appropriate check
procedures before each sampling run. A suitable procedure for control of leakage is given in Annex A. The
leak check shall be carried before and after sampling.
6.5 Handling, storage, transport of sampled tubes
6.5.1 General
Containers and materials emitting (outgasing) VOC, e.g. wood, certain plastics and sealing tape, shall not be
used for sample storage and transport.
If sampled tubes cannot be analysed within 7 days they shall be stored in an air-tight container at < 4 °C
(refrigerated)
All tubes stored under refrigerated conditions, shall be allowed to equilibrate with room temperature before
they are removed from their storage container and uncapped for analysis. Allowing the tubes to equilibrate
with room temperature prevents ambient humidity condensing inside cold tubes.
6.5.2 Activated carbon (charcoal) tubes
Sampled tubes shall be capped then stored and transported in an airtight VOC free container without
exposure to direct sunlight and below 20 °C.
6.5.3 Thermal desorption tubes
Thermal desorption tubes shall be sealed using long term storage caps before and immediately after sampling
as specified in EN ISO 16017-1 (Subclause 6.2). Once capped, sorbent thermal desorption tubes shall be
stored and transported in a VOC free air-tight container without exposure to direct sunlight and below
20 °C.
If sampled thermal desorption tubes are stored under refrigerated conditions, caps shall be retightened after
the tubes have reached their minimum storage temperature.
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6.6 Blanks
6.6.1 Field blanks
Field blank tubes comprise conditioned sorbent tubes, taken from the same batch as those used for field
monitoring and handled in the same manner at the sample location as the sampling tubes but which are not
exposed to the waste gas stream or fitted into the sample train. They are subsequently analysed with the
sampled tubes to determine the average blank level for each compound of interest.
Every measurement campaign shall include at least one field blank per day. When taking more than 6
samples in one day then 2 field blanks are required. For greater than 10 samples in one day then 3 field
blanks are required.
In the case of activated carbon tubes it is only necessary to analyse the main adsorption layer of any field or
analytical blank.
6.6.2 Analytical (laboratory) blanks
Analytical (laboratory) blanks comprise conditioned samplers (sorbent tubes), taken from the same batch as
those used for field monitoring, but which are retained, capped and sealed in the laboratory throughout the
monitoring exercise. They shall be subsequently analysed with the sampled tubes as a check on inherent
sampler cleanliness (see 5.3) and the level of background contamination of the analytical system.
7 Analytical procedure
7.1 Calibration of the GC analysis
7.1.1 GC calibration for analysis of solvent extracts
Calibration solutions shall be prepared using the same extraction solvent that is used for the sample tubes.
The range of concentration of the calibration solutions shall cover the concentrations of the sample extracts
to be analysed (see 5.6.3). At least five different concentration levels shall be used for calibration.
NOTE 1 Calibration solutions with low concentrations of organic compounds can be prepared by first making a stock
solution and then by diluting the stock solution to various concentrations. However, extraction solvents are highly
volatile and evaporative losses should be minimised by using vessels closed with septa. The amount of the evaporative
losses can be determined by weighing the vessels before adding the first organic compound to the extraction agent
and after adding the last organic compound to the desorption agent. The least volatile organic compound should be
added to the extraction solvent first and the most volatile organic compound should be added last. The
evaporative losses are the difference between theoretical final weight and real final weight and should be less than 1 % of
the theoretical final weight.
NOTE 2 Typically 1 µl of each calibration solution should be injected into the GC, operating under the same conditions
as for the sample analysis, three times. A calibration graph should be prepared for every organic compound by plotting
the area of the compound peaks, corrected for blank levels of the extraction solvent, on the vertical scale against the
mass of the compound, in micrograms, corresponding to the concentration in the calibration solutions.
NOTE 3 The calibration equation should be determined using linear regression:
A = f ⋅m +b
i i i i
where
A is the measured area of organic component i
i
f is the slope of the calibration line for organic component i
i
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m is the mass of organic component i
...
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