SIST EN 12619:2013
(Main)Stationary source emissions - Determination of the mass concentration of total gaseous organic carbon - Continuous flame ionisation detector method
Stationary source emissions - Determination of the mass concentration of total gaseous organic carbon - Continuous flame ionisation detector method
The method specified in this European Standard is designed for use as a standard reference method.This European Standard specifies a set of minimum performance requirements for an instrument using flame ionization detection, together with procedures for its calibration and operation, for the measurement of the mass concentration of total gaseous organic carbon (TOC) and for solvent emissions total volatile organic compounds (TVOC) in stationary source emissions.This European Standard is suitable for the measurement of gaseous or vapour phase TOC and TVOC emissions such as emissions from waste incinerators and solvent using processes.The results obtained using this standard, are expressed in milligrams per cubic metre as total carbon (mg/m3). This standard is suitable for use in the range 1 mg/m3 up to at least 1000 mg/m3.This European Standard is not applicable for permanently installed AMS. For permanently installed AMS refer to EN15267-3.
Emissionen aus stationären Quellen - Bestimmung der Massenkonzentration des gesamten gasförmigen organisch gebundenen Kohlenstoffs - Kontinuierliches Verfahren mit dem Flammenionisationsdetektor
Das in dieser Europäischen Norm festgelegte Verfahren ist für die Anwendung als Standardreferenzverfahren konzipiert.
Diese Europäische Norm legt einen Satz von Mindestanforderungen für ein Messgerät mit Flammenioni-sations¬detektion sowie die Vorgehensweise bei Kalibrierung und Betrieb dieses Geräts zur Messung der Massen¬konzentration des gesamten gasförmigen organisch gebundenen Kohlenstoffs (TOC) und der aus Lösemitteln stammenden gesamten flüchtigen organischen Verbindungen (TVOC) in Emissionen aus stationären Quellen fest.
Diese Europäische Norm ist für die Messung von gas- und dampfförmigen TOC- und TVOC-Emissionen, z. B. aus Müllverbrennungsanlagen oder aus Lösemittel verwendenden Prozessen, geeignet.
Die nach dieser Norm ermittelten Ergebnisse werden als Gesamtkohlenstoff in Milligramm je Kubikmeter (mg/m3) angegeben. Diese Norm ist für den Bereich von 1 mg/m3 bis mindestens 1 000 mg/m3 geeignet.
Diese Norm ist nicht für fest installierte AMS geeignet. Für diese gilt EN 15267-3.
ANMERKUNG Dieses Verfahren kann auch für höhere Massenkonzentrationen an TVOC angewendet werden.
Emissions de sources fixes - Détermination de la concentration massique en carbone organique total - Méthode du détecteur continu à ionisation de flamme
La méthode spécifiée dans la présente Norme européenne est conçue pour être utilisée comme méthode de référence normalisée.
La présente Norme européenne spécifie un ensemble d’exigences de performances minimales ainsi que les modes opératoires d’étalonnage et de fonctionnement d’un appareil utilisant la détection à ionisation de flamme pour mesurer la concentration massique en carbone organique total gazeux (COT) et pour les composés organiques volatiles totaux (COVT) des émissions de solvants, dans les émissions de sources fixes.
La présente Norme européenne est adaptée à la mesure des émissions de COT et COVT en phase gazeuse ou vapeur telles que les émissions provenant des incinérateurs de déchets et des process utilisant des solvants.
Les résultats obtenus en utilisant la présente norme sont exprimés en milligrammes par mètre cube de carbone total (mg/m³). La présente norme est utilisable sur une plage allant de 1 mg/m³ à au moins 1000 mg/m³.
La présente Norme européenne ne s’applique pas aux AMS installés en permanence. Pour les AMS installés en permanence, se référer à l’EN 15267-3.
NOTE La présente méthode peut également être utilisée pour des concentrations massiques supérieures de COVT.
Emisije nepremičnih virov - Določevanje masnih koncentracij celotnega organskega ogljika v plinasti fazi - Kontinuirana metoda plamenske ionizacijske detekcije
Metoda iz tega evropskega standarda je namenjena za uporabo kot standardna referenčna metoda. Ta evropski standard določa sklop minimalnih zahtev za delovanje instrumenta, ki uporablja plamensko ionizacijsko detekcijo, skupaj s postopki za njegovo umerjanje in upravljanje, za merjenje masne koncentracije celotnega organskega ogljika v plinasti fazi (TOC) in za emisije topil celotnih hlapnih organskih spojin (TVOC) v emisijah nepremičnih virov. Ta evropski standard je primeren za merjenje emisij celotnega organskega ogljika in celotnih hlapnih organskih spojin v plinasti ali parni fazi, kot so emisije iz sežigalnic odpadkov in procesov na podlagi topil. Rezultati, pridobljeni v skladu s tem standardom, so izraženi v miligramih na kubični meter kot skupni ogljik (mg/m3). Ta standard je primeren za uporabo v razponu 1 mg/m3 do najmanj 1000 mg/m3. Ta evropski standard se ne uporablja za trajno vgrajene avtomatske merilne sisteme (AMS). Za trajno vgrajene AMS glej standard EN 15267-3.
General Information
Relations
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.QHJDGHWHNFLMHEmissionen aus stationären Quellen - Bestimmung der Massenkonzentration des gesamten gasförmigen organisch gebundenen Kohlenstoffs - Kontinuierliches Verfahren mit dem FlammenionisationsdetektorEmissions de sources fixes - Détermination de la concentration massique en carbone organique total - Méthode du détecteur continu à ionisation de flammeStationary source emissions - Determination of the mass concentration of total gaseous organic carbon - Continuous flame ionisation detector method13.040.40Stationary source emissionsICS:Ta slovenski standard je istoveten z:EN 12619:2013SIST EN 12619:2013en,fr,de01-april-2013SIST EN 12619:2013SLOVENSKI
STANDARDSIST EN 13526:2002SIST EN 12619:20001DGRPHãþD
SIST EN 12619:2013
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 12619
January 2013 ICS 13.040.40 Supersedes EN 12619:1999, EN 13526:2001English Version
Stationary source emissions - Determination of the mass concentration of total gaseous organic carbon - Continuous flame ionisation detector method
Emissions de sources fixes - Détermination de la concentration massique en carbone organique total - Méthode du détecteur continu à ionisation de flamme
Emissionen aus stationären Quellen - Bestimmung der Massenkonzentration des gesamten gasförmigen organisch gebundenen Kohlenstoffs - Kontinuierliches Verfahren mit dem Flammenionisationsdetektor This European Standard was approved by CEN on 24 November 2012.
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. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member.
This European Standard exists 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, 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
Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2013 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 12619:2013: ESIST EN 12619:2013
EN 12619:2013 (E) 2 Contents Page Foreword . 3 1 Scope . 4 2 Normative references . 4 3 Terms and definitions . 4 4 The principle of the technique . 6 5 Requirements for apparatus and gases . 7 6 Measurement procedure . 9 Annex A (normative)
Determination of the performance characteristics of a FID . 12 Annex B (informative)
Basic functionality of an FID . 15 Annex C (informative)
Measurement uncertainty and associated statistics . 18 Annex D (informative)
Safety measures . 20 Annex E (informative)
Significant technical changes . 21 Bibliography. 22
SIST EN 12619:2013
EN 12619:2013 (E) 3 Foreword This document (EN 12619:2013) has been prepared by Technical Committee CEN/TC 264 “Air quality”, the secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by July 2013, and conflicting national standards shall be withdrawn at the latest by July 2013. 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 12619:1999 and EN 13526:2001. The list of the most significant technical changes that have been made in this new edition is to be found in Annex E. According to the CEN/CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard: 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. SIST EN 12619:2013
EN 12619:2013 (E) 4 1 Scope This European Standard specifies a flame ionisation detector (FID) method. It is intended for use as a standard reference method for the measurement of the mass concentration of gaseous and vaporous organic substances (expressed as TVOC) in stationary source emissions (e.g. emissions from waste incinerators and solvent using processes, emission measurements according to 2010/75/EU) in the concentration range up to 1 000 mg/m³.
This European Standard specifies the requirements for an instrument using flame ionisation detection, together with procedures for its operation. The results obtained using this standard are expressed in milligrams per cubic metre (mg/m³) as total carbon (TVOC). This European Standard is not applicable for permanently installed automated measuring systems (AMS). Alternative methods to this method may be used provided that the user can demonstrate equivalence, based on the principles of CEN/TS 14793. 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 15267-1, Air quality — Certification of automated measuring systems — Part 1: General principles EN 15267-2, Air quality — Certification of automated measuring systems — Part 2: Initial assessment of the AMS manufacturer’s quality management system and post certification surveillance for the manufacturing process EN 15267-3:2007, Air quality — Certification of automated measuring systems — Part 3: Performance criteria and test procedures for automated measuring systems for monitoring emissions from stationary sources EN ISO 9169, Air quality — Definition and determination of performance characteristics of an automatic measuring system (ISO 9169) EN ISO 14956, Air quality — Evaluation of the suitability of a measurement procedure by comparison with a required measurement uncertainty (ISO 14956) 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 combustion air air supply used for the combustion of fuel gas in an instrument using flame ionisation detection 3.2 detection limit minimum concentration of a substance which produces an observable response, which is two times the standard deviation at zero SIST EN 12619:2013
EN 12619:2013 (E) 5 3.3 dilution gas gas used to dilute sampled flue gas to prevent water condensation 3.4 flame ionisation detector (FID) instrument using flame ionisation detection 3.5 flue gas product from a combustion, incineration or solvent process containing gaseous and/or particulate compounds 3.6 fuel gas gas of known composition used to maintain the flame of the FID 3.7 mass concentration of gaseous total organic carbon quotient of the mass of total organic carbon to the volume of the dry gas under specified reference conditions of temperature and pressure, normally expressed in milligrams per cubic metre (mg/m3) as total carbon 3.8 residence time time period for the sampled gas to be transported from the inlet of the probe to the inlet of the measurement cell 3.9 response factor dimensionless quotient of the response of the FID with any carbon based compound or compounds to its response to propane, in each case referred to the number of carbon atoms of the molecule 3.10 response time time which elapses between the moment when a change is produced and the moment when the instrument response reaches a value of 90 % of the final change in instrument response as a consequence of a stepwise change in the total organic carbon concentration 3.11 span gas test gas used to check and adjust a specific point on a calibration curve 3.12 total volatile organic carbon (TVOC) total volatile organic compounds which are measured by the FID, expressed in milligrams per cubic metre (mg/m3) as total carbon 3.13 zero gas test gas used to check and adjust the zero point on a calibration curve 3.14 uncertainty parameter associated with the result of a measurement, that characterises the dispersion of the values that could reasonably be attributed to the measurand [SOURCE: ENV 13005] SIST EN 12619:2013
EN 12619:2013 (E) 6 4 The principle of the technique 4.1 Flame ionisation detector (FID) The measurement technique utilised by the flame ionisation detector (FID) is the ionisation of organically bound carbon atoms in a hydrogen flame. The ionisation current measured by the FID depends on the number of C-atoms of organic compounds burning in the fuel gas flame, the form of bonding (straight chain or branched chain) and of bonding partners. The response factor is a function of the specific design of the detector and the adjusted operating conditions. The advantage of the FID is that it responds to organic carbon compounds and has negligible response to inorganic flue gas compounds (such as CO, CO2, NO, H2O). A number of different instrument configurations exist. Figure 1 is an example of the principle whereby in the detector a sample gas is fed into a hydrogen flame across which a DC electrical potential is placed. The introduction of the sampled gas causes a specific ionisation current to flow, which is measured using suitable equipment. Defined test gases are required to determine the response factors. These can be produced by a number of methods including: static methods (with gas collectors or direct injection) or dynamic methods (e.g. vapour pressure method or certified test gases from compressed gas bottles). The span of the instrument shall be adjusted with propane (C3H8) for which the response factor, defined in this standard, has been set at 1,00. The final value will be expressed as TVOC in milligrams per cubic metre. Refer to Annex B for more information on the use and effects of an FID instrument.
Key 1 polarisation voltage 6 fuel gas 2 electrodes 7 sample gas 3 ions 8 jet 4 flame 9 amplifier and readout 5 combustion air Figure 1 — Principle of FID SIST EN 12619:2013
EN 12619:2013 (E) 7 4.2 Sampling and sampling device Sampling is the process of extracting from the flue gas a partial volume flow which is representative of the composition of the main gas stream. A partial flow of the flue gas is directly fed into the FID analyser via the sampling probe, the particle filter and the heated sampling line. An example of the set-up of the measuring system is shown in Figure 2. The sampling device including the filter needed to remove fine particles, which could clog the burner, is heated to avoid sample condensation.
Key 1 sampling probe 6 bypass (optional) 2 zero and span gas inlet 7 test gas inlet for functional tests 3 particle filter, heated 8 FID 4 sampling line, heated 9 data evaluation system 5 external sample pump (optional), heated
Figure 2 — Example of the set-up of the measuring system 5 Requirements for apparatus and gases 5.1 Requirements for the measurement system The sampling system shall meet the following requirements:
It shall be made of stainless steel, polytetrafluoroethylene or polypropylenefluoride. If an alternative material is used, it shall be proven that it is chemically and physically inert to the constituents of the flue gas under analysis. The design and configuration of the sampling device used shall ensure the residence time of the sample gas within the device is minimised in order to reduce the response time of the measuring system. It will be designed to ensure a sample residence time less than 60 s. With long sampling lines or high flow resistance, the use of an external pump with bypass is recommended. It shall be heated throughout to at least 180 °C. NOTE Sampling lines in PTFE have a maximum temperature of 200 °C. All instruments that are certified are tested at 180 °C. It shall have a heated filtering device upstream of the sampling line to trap all particles liable to impair the operation of the apparatus. It shall have an inlet for applying zero and span gases at or close to the probe inlet of the sampling probe, upstream of the filter. This is to check the sampling system including the filter assembly. The FID and sampling system shall comply with the performance requirements of EN 15267-3. SIST EN 12619:2013
EN 12619:2013 (E) 8 The checks in Table 1 shall be carried out with at least the specified frequency. Table 1 — Minimum frequency of checks for QA/QC during the operation Check Minimum frequency Requirement Clause Response time once for each measurement series ≤ 200 s A.2 Repeatability standard deviation at zero point once a year ≤ 2 % A.4 Repeatability standard deviation at span point once a year ≤ 2 % A.5 Lack of fit once a year and after repair a of the instrument ≤ 2 % A.3 Effect of oxygen at least once a year and after repair (can be carried out by the manufacturer) ≤ 2 % A.6 Other interference checks b at least once a year and after repair (can be carried out by the manufacturer) ≤ 2 % A.7 Response factor determination as specified by the manufacturer and is relevant for single compound measuring tasks
A.8 and Annex B Sampling system check once for each measurement series
6.2.2 Leakage check once for each measurement series
6.2.2 Zero drift at the beginning and end of the measuring period and at least once a day < 5 % 6.2.3 Span drift at the beginning and end of the measuring period and at least once a day < 5 % 6.2.3 Regular maintenance of the analyser as required by the manufacturer
Cleaning or changing of sampling line and particulate filters c once for each measurement series, if needed
a A repair that might affect the performance of the instrument. b Only those interferences shall be checked which have proven to be relevant during instrument performance testing. c The particulate filter shall be changed periodically depending on the dust load at the sampling site. During this filter change, the filter housing shall be cleaned. 5.2 Operational gases 5.2.1 General A number of operational gases are required when using this standard. The use of combustion air or fuel gas whose concentration in TVOC is lower than 0,2 mg/m³ (as carbon) or of purity 99,998 % shall be used. This avoids any risk of influence of this gas on the result of the measurement. 5.2.2 Fuel gases The fuel gas shall be specified by the equipment manufacturer and according to the certification to EN 15267-1, EN 15267-2 and EN 15267-3. Commonly used gases include: hydrogen; hydrogen/helium mixture;
SIST EN 12619:2013
EN 12619:2013 (E) 9 hydrogen/nitrogen mixture. NOTE The fuel gas pipe will be made from a suitable material for the environment, e.g. stainless steel, copper or PTFE. 5.2.3 Zero gas The TVOC concentration (mg/m3 as carbon) of zero gas shall be lower than 0,2 mg/m3 of carbon or purity 99,998 % shall be used. This avoids any risk of influence of this gas on the result of the measurement. This can be synthetic air or cleaned ambient air. If a problem occurs at the zero point e.g. negative values, this may be an indication of the effect of oxygen. In this case, it is recommended the zero gas may be replaced with one containing a similar oxygen concentration to the process (nitrogen/oxygen mixture or synthetic air). The worst case for this effect is when a process is running with approximately 10 % excess oxygen. Refer to Annex B for more information on the use and effects of an FID instrument. 5.2.4 Span gas The span gas shall be propane in synthetic air or in a nitrogen/oxygen mixture. It shall have a known concentration of TVOC and the expanded uncertainty on the analytical certificate of the span gas shall be less than or equal to 2 % for TVOC.
When the analyser is used for regulatory purposes, the span gas shall have a known concentration of approximately the half-hourly ELV or 50 % to 90 % of the selected range of the analyser. The span gas will be propane with the same oxygen concentration in the complementary gas in the zero and in the span gas to take into account the same level of influence at the zero point and the span point during the adjustment of the analyser. 6 Measurement procedure 6.1 General The planning and sampling strategy shall follow the requirements of EN 15259. The following text describes the routine operation procedures required by the standard; a more detailed procedure for determining the instrument performance characteristics is given in Annex A. 6.2 Adjustments and checks 6.2.1 Instrument adjustment The FID shall be set up according to the manufacturer's instructions in order to ensure that the instrument is correctly adjusted as specified in Table 1. At the beginning of the measuring period, zero and span gases are supplied to the analyser directly, without passing through the sampling system. Adjustments are made until the correct zero and span gas values are given by the data sampling system:
adjust the zero value; adjust the span; finally, re-check zero to see if there are no significant changes (zero deviation lower than two times the repeatability at zero). Repeat the adjustment procedure until this is achieved. SIST EN 12619:2013
EN 12619:2013 (E) 10 6.2.2 Check of the sampling system Before starting the measurement, the following procedure shall be applied to determine if there is leakage and or impurities in the sampling line: Zero and span gas are supplied to the analyser through the sampling system, as close as possible to the probe inlet (in front of the filter). Any differences between the readings obtained during the adjustment of the analyser (6.2.1) and during the check of the sampling system shall be lower than 2 % of the span value. NOTE Differences may be due to leakage or impurities in the sampling system leading to memory effects due to adsorption or desorption to or from the surfaces. Check also the response time of the system. 6.2.3 Zero and span checks after measurement At the end of the measuring period and at least once a day, zero and span checks shall be performed at the inlet of the sampling system by supplying test gases. If the span or zero drifts are bigger than 2 % of the span value, it is necessary to correct both for zero and span drifts. Values shall be recorded before any adjustments to the analyser. NOTE Recorded values can be used for uncertainty calculations. The drift of zero and span shall be lower than 5 % of the span value; otherwise, the
...
SLOVENSKI STANDARD
oSIST prEN 12619:2011
01-maj-2011
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Stationary source emissions - Determination of the mass concentration of total gaseous
organic carbon - Continuous flame ionisation detector method
Emissionen aus stationären Quellen - Bestimmung der Massenkonzentration des
gesamten gasförmigen organisch gebundenen Kohlenstoffs - Kontinuierliches Verfahren
mit dem Flammenionisationsdetektor
Emissions de sources fixes - Détermination de la concentration massique en carbone
organique total - Méthode du détecteur continu à ionisation de flamme
Ta slovenski standard je istoveten z: prEN 12619
ICS:
13.040.40 (PLVLMHQHSUHPLþQLKYLURY Stationary source emissions
oSIST prEN 12619:2011 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN 12619:2011
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oSIST prEN 12619:2011
EUROPEAN STANDARD
DRAFT
prEN 12619
NORME EUROPÉENNE
EUROPÄISCHE NORM
January 2011
ICS 13.040.40 Will supersede EN 12619:1999, EN 13526:2001
English Version
Stationary source emissions - Determination of the mass
concentration of total gaseous organic carbon - Continuous
flame ionisation detector method
Emissions de sources fixes - Détermination de la Emissionen aus stationären Quellen - Bestimmung der
concentration massique en carbone organique total - Massenkonzentration des gesamten gasförmigen
Méthode du détecteur continu à ionisation de flamme organisch gebundenen Kohlenstoffs - Kontinuierliches
Verfahren mit dem Flammenionisationsdetektor
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 12619:2011: E
worldwide for CEN national Members.
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oSIST prEN 12619:2011
prEN 12619:2011 (E)
Contents Page
Foreword .3
1 Scope .4
2 Normative references .4
3 Terms and definitions .5
4 The principle of the technique .6
5 Apparatus and gases .8
6 Measurement procedure . 10
Annex A (normative) Determination of the performance characteristics of a FID . 13
Annex B (informative) Basic functionality of an FID . 16
Annex C (informative) Safety measures. 19
Annex D (informative) Significant technical changes . 20
Bibliography . 21
2
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oSIST prEN 12619:2011
prEN 12619:2011 (E)
Foreword
This document (prEN 12619:2011) 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 13526:2001, EN 12619:1999.
3
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oSIST prEN 12619:2011
prEN 12619:2011 (E)
1 Scope
The method specified in this European Standard is designed for use as a standard reference method.
This European Standard specifies a set of minimum performance requirements for an instrument using flame
ionization detection, together with procedures for its calibration and operation, for the measurement of the
mass concentration of total gaseous organic carbon (TOC) and for solvent emissions total volatile organic
compounds (TVOC) in stationary source emissions.
This European Standard is suitable for the measurement of gaseous or vapour phase TOC and TVOC
emissions such as emissions from waste incinerators and solvent using processes.
The results obtained using this standard, are expressed in milligrams per cubic metre as total carbon (mg/m³).
This standard is suitable for use in the range 1 mg/m³ up to at least 1000 mg/m³.
This European Standard is not applicable for permanently installed AMS. For permanently installed AMS refer
to EN 15267-3.
NOTE This method can also be used also for higher mass concentrations TVOC.
2 Normative references
This European Standard incorporates, by dated or undated reference, provisions from other publications.
These normative references are cited at the appropriate places in the text and the publications are listed
hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to
this European Standard only when incorporated in it by amendment or revision. For undated references the
latest edition of the publication referred to applies.
EN 14789, Stationary source emissions — Determination of volume concentration of oxygen (O2) —
Reference method — Paramagnetism
EN 14790, Stationary source emissions — Determination of the water vapour in ducts
EN 15259, Air quality — Measurement of stationary source emissions — Requirements for measurement
sections and sites and for the measurement objective, plan and report
EN 15267-3, Air quality — Certification of automated measuring systems — Part 3: Performance criteria and
test procedures for automated measuring systems for monitoring emissions from stationary sources
ENV 13005, Guide to the expression of uncertainly in measurement
EN ISO 14956, Air Quality — Evaluation of the suitability of a measurement procedure by comparison with a
required measurement uncertainty
CEN/TS 14793, Stationary source emissions — Interlaboratory validation procedure for an alternative method
compared to a reference method
4
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oSIST prEN 12619:2011
prEN 12619:2011 (E)
3 Terms and definitions
For the purposes of this standard, the following definitions apply.
3.1
combustion air
air supply used for the combustion of fuel gas in an instrument using flame ionization detection
3.2
complementary gas
component of a calibration gas which completes a calibration gas mixture
3.3
control gas mixture
gas mixture used to check the minimum performance requirements of the FID during instrument certification
3.4
detection limit
minimum concentration of a substance which produces an observable response, as detailed in A.1.2 and
referred to in ISO 7504:1984
3.5
dilution gas
gas used to dilute sampled flue gas to prevent water condensation
3.6
flame ionization detector (FID)
instrument using flame ionisation detection
3.7
flue gas
product from a combustion, incineration or solvent process containing gaseous and/or particulate components
3.8
fuel gas
gas of known composition used to maintain the flame of the FID
3.9
mass concentration of gaseous total organic carbon
quotient of the mass of total organic carbon to the volume of the dry gas under specified reference
conditions of temperature and pressure, normally expressed in milligrams per cubic metre as total carbon
(mgC/m³)
3.10
residence time
time period for the sampled gas to be transported from the inlet of the probe to the inlet of the measurement
cell
3.11
response factor
dimensionless quotient of the response of the FID with any carbon based compound or compounds to
its response to propane, in each case referred to the number of carbon atoms of the molecule
3.12
response time
time which elapses between the moment when a change is produced and the moment when the instrument
response reaches a value of 90 % of the final change in instrument response as a consequence of a stepwise
5
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change in the total organic carbon concentration
3.13
span gas
gas used to adjust and check a specific point on a calibration curve
3.14
total organic carbon (TOC)
by convention the total gaseous organic carbon which is measured by the FID and expressed as mgC/m³
3.15
total volatile organic carbon (TVOC)
by convention total volatile organic compounds which are measured by the FID, expressed as mgC/m³ from
solvent using process
3.16
zero gas
gas or a gas mixture used to check and adjust the zero point on a calibration curve
3.17
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
3.18
uncertainty
parameter associated with the result of a measurement, that characterizes the dispersion of the values that
could reasonably be attributed to the measurand
3.19
uncertainty budget
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
3.20
overall uncertainty
expanded combined standard uncertainty attached to the measurement result calculated according to
ENV 13005
4 The principle of the technique
4.1 Flame ionization detector (FID)
The measurement technique utilized by the FID is the ionization of organically bound carbon atoms in a
hydrogen flame. The ionization current measured by the FID depends on the number of C-atoms of organic
compounds burning in the fuel gas flame, the form of bonding (straight chain or branched chain) and of
bonding partners.
The response factor is a function of the specific design of the detector and the adjusted operating conditions.
The advantage of the FID is that it responds to organic carbon compounds and has negligible response to
inorganic flue gas compounds (such as CO, CO , NO, H O).
2 2
A number of different instrument configurations exist. Figure 1 is an example of the principle whereby in the
detector a sample gas is fed into a hydrogen flame across which a DC electrical potential is placed. The
introduction of the sampled gas causes a specific ionization current to flow, which is measured using suitable
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equipment. Defined test gases are required to determine the response factors. These can be produced by a
number of methods including: static methods (with gas collectors or direct injection) or dynamic methods (e.g.
vapour pressure method or certified test gases from compressed gas bottles).
The span of the instrument shall be adjusted with propane (C H ) for which the response factor, defined in this
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standard, has been set at 1,00. The final value will be expressed as TOC in milligrams per cubic metre.
Refer to Annex B for more information on the use and effects of an FID instrument.
Key
1 polarisation voltage 6 fuel gas
2 electrodes 7 sample gas
3 ions 8 jet
4 flame 9 amplifier and readout
5 combustion air
Figure 1 — Principle of FID
4.2 Sampling and sampling device
Sampling is the process of extracting from a large quantity of flue gas a small portion which is truly
representative of the composition of the main gas stream.
A partial flow of the flue gas is directly fed into the FID analyser via the sampling probe, the particle filter and
the heated sampling line. An example of the set-up of the measuring system is shown in Figure 2. The
sampling device including the filter needed to remove fine particles, which could clog the burner, is heated to
avoid sample condensation.
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Key
1 sampling probe 6 bypass (optional)
2 zero and span gas inlet 7 test gas inlet for functional tests
3 particle filter (in-stack or out-stack), heated 8 FID
4 sampling line, heated 9 data evaluation system
5 external sample pump (optional), heated
Figure 2 — Example of the set-up of the measuring system
5 Apparatus and gases
5.1 Sampling device
The sampling device shall meet the following requirements:
It shall be made of stainless steel, polytetrafluoroethylene or polypropylenefluoride. If an alternative
material is used, it shall be proven by validation that it is chemically and physically inert to the
constituents of the flue gas under analysis.
NOTE 1 If a material is used in a permanently installed FID AMS with type approval to EN 15267-3, then it can be
assumed that the material will be acceptable for use in a portable version of the AMS.
The design and configuration of the sampling device used shall ensure the residence time of the sample
gas within the device is minimised in order to reduce the response time of the measuring system.
NOTE 2 It should be designed to ensure a sample residence time less than 60 s; with long sampling lines or high flow
resistance the use of an external pump with bypass is recommended.
It shall be heated throughout to at least 180 °C.
NOTE 3 Sampling lines in PTFE has a maximum temperature of 200 °C.
It shall have a heated filtering device upstream of the sampling line to trap all particles liable to impair the
operation of the apparatus;
It shall have an inlet for applying zero and span gases at or close to the probe inlet of the sampling probe,
upstream of the filter. This is to check the sampling system including the filter assembly.
5.2 The FID
The FID and sampling system shall comply with the performance requirements of EN 15267-3.
5.3 Periodic and annual checks
The periodic and annual checks in Table 1 shall be carried out.
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Table 1 — Minimum frequency of checks for QA/QC during the operation
Check Minimum frequency
Response time The response time will be controlled periodical
Repeatability standard deviation at zero once a year
point
Repeatability standard deviation at span once a year
point
Lack of fit once a year and after repair of the instrument
Effect of oxygen at least once a year and after repair (can be carried
out by the manufacturer)
Other interference checks once a year and after repair (can be carried out by the
manufacturer)
Sampling system and leakage check once for each measurement series
a
once for each measurement series, if needed
Cleaning or changing of particulate filters
at the sampling inlet and at the monitor inlet
Zero drift at the beginning and end of the measuring period and
at least once a day
Span drift at the beginning and end of the measuring period and
at least once a day
Regular maintenance of the analyser as required by the manufacturer
a
The particulate filter shall be changed periodically depending on the dust load at the sampling site. During this filter change
the filter housing shall be cleaned.
5.4 Operational gases
A number of operational gases are required when using the standard.
NOTE The use of combustion air or fuel gas whose concentration in TOC is lower than 0,2 mgC/m³ or of purity
99,998 % is recommended and allows to avoid any risk of influence of this gas on the result of the measurement.
5.4.1 Combustion air
The TOC concentration (mgC/m³) of combustion air shall not exceed 1 % of the emission limit value (ELV)
TOC. This can be synthetic air or cleaned ambient air.
5.4.2 Fuel gases
The fuel gas shall be specified by the equipment manufacturer, it may be:
hydrogen;
hydrogen/helium mixture;
hydrogen/nitrogen mixture.
The TOC concentration (mgC/m³) of fuel gas shall not exceed 1 % of the emission limit value (ELV) TOC. This
can be synthetic air or cleaned ambient air.
NOTE 1 Gases with a purity of 99,999 % (percent by volume) usually meet this requirement.
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NOTE 2 The fuel gas pipe should be made from stainless steel or copper.
5.4.3 Zero gas
The TOC concentration (mgC/m³) of zero gas shall not exceed 1 % of the emission limit value (ELV) TOC.
This can be Synthetic air or cleaned ambient air.
NOTE 1 If a problem occurs at the zero point, e.g. negative values, this may be an indication of the effect of oxygen. In
this case it is recommended the zero gas may be replaced with one containing a similar oxygen concentration to the
process (nitrogen, nitrogen/oxygen mixture or synthetic air). Worst case for this effect is when a process is running with
approx 10 % excess oxygen. Refer to Annex B for more information on the use and effects of an FID instrument.
NOTE 2 Cleaning ambient air with charcoal, will not remove methane and ethane. Therefore, charcoal filtered air
cannot be used as zero gas.
5.4.4 Span gas
The span gas shall be propane in synthetic air. It shall have a known concentration of TOC and the
uncertainty on the analytical certificate of the span gas shall be less than or equal to ± 2 % for TOC.
When the analyser is used for regulatory purposes, the span gas shall have a known concentration of
approximately the half-hourly ELV or 50 % to 90 % of the selected range of the analyser.
6 Measurement procedure
Planning and sampling strategy shall follow the requirements of EN 15259.
The following text describes the routine operation procedures required by the standard, a more detailed
procedure for determining the instrument performance characteristics is given in Annex A.
6.1 Adjustments and checks
6.1.1 Instrument adjustment
The FID shall be set
...
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