SIST-TS CEN/TS 16429:2013
(Main)Stationary source emissions - Sampling and determination of hydrogen chloride content in ducts and stacks - Infrared analytical technique
Stationary source emissions - Sampling and determination of hydrogen chloride content in ducts and stacks - Infrared analytical technique
This Technical Specification specifies an automatic method for determination of the mass concentration of hydrogen chloride (HCl) in ducts and stacks emitting to atmosphere. It describes the infrared analytical technique, including the sampling and gas conditioning system. The method should fulfil the performance characteristics requirements of this Technical Specification and the expanded uncertainty is less than 20 % relative at the daily Emission Limit Value (ELV). In order to use an alternative method to this method, it is necessary to demonstrate equivalence according to the Technical Specification CEN/TS 14793. It is necessary that the capability to demonstrate equivalence is officially recognised by the national accreditation body or law.
Emissionen aus stationären Quellen - Probenahme und Bestimmung von Chlorwasserstoff in Abgaskanälen und -kaminen - Infrarotverfahren
Diese Technische Spezifikation legt ein automatisches Verfahren zur Bestimmung der Massenkonzentration von Chlorwasserstoff (HCl) in Abgasen, die aus Kanälen und Kaminen in die Atmosphäre emittiert werden, fest. Sie beschreibt das Infrarotverfahren, einschließlich der Einrichtungen zur Probenahme und Gaskonditionierung. Das Verfahren muss die in dieser Technischen Spezifikation festgelegten Anforderungen an Leistungskenngrößen erfüllen, und die Gesamtunsicherheit des Verfahrens muss kleiner als 20 % (relativ) beim 1-Tages-Emissionsgrenzwert (ELV) sein. Wenn das IR-Verfahren in einer fest im Abgaskamin eingebauten automatischen Messeinrichtung angewendet wird, sind EN 14181 und andere relevante Normen des CEN/TC 264 maßgeblich. Um anstelle dieses Verfahrens ein alternatives Verfahren einzusetzen, ist dessen Gleichwertigkeit nach der Technischen Spezifikation CEN/TS 14793 nachzuweisen. Die Befähigung zum Nachweis der Gleichwertigkeit muss von der nationalen Akkreditierungsstelle oder gesetzlich anerkannt sein.
Émissions de sources fixes - Prélèvement et détermination du chlorure d'hydrogène dans les conduits et les cheminées - Technique analytique infrarouge
La présente Spécification technique décrit une méthode de détermination automatique de la concentration massique de chlorure d'hydrogène (HCl) émis dans l'atmosphère par les conduits et les cheminées. Elle décrit la technique analytique infrarouge, y compris le système de prélèvement et de conditionnement du gaz. La méthode doit satisfaire aux exigences relatives aux caractéristiques de performance de la présente Spécification technique et l'incertitude globale de la méthode est inférieure à la valeur relative de 20 % à la valeur limite d'émission journalière (VLE).
Si une technique infrarouge est employée comme système automatique de mesurage (AMS) installé à demeure sur une cheminée, se référer à l'EN 14181 et aux autres normes pertinentes rédigées par le CEN/TC 264.
Pour utiliser une variante à la présente méthode, il est nécessaire d'en démontrer l'équivalence selon la Spécification technique CEN/TS 14793. La capacité à démontrer l'équivalence doit être officiellement reconnue par l'organisme national d'accréditation ou la loi.
Emisije nepremičnih virov - Vzorčenje in določevanje vodikovega klorida v odvodnikih in odvodnikih v zrak - Infrardeča analizna tehnika
Ta tehnična specifikacija določa samodejno metodo za določevanje masne koncentracije vodikovega klorida (HCl) v odvodnikih in odvodnikih v zrak, ki uhaja v ozračje. Opisuje infrardečo analizno tehniko, vključno s sistemom za vzorčenje in kondicioniranje plinov. Metoda naj bi izpolnjevala zahteve glede karakteristik delovanja te tehnične specifikacije, pri čemer je razširjena negotovost manj kot 20 % relativna pri dnevni mejni vrednosti emisij (ELV). Da bi se namesto te metode uporabila alternativna metoda, je treba dokazati enakovrednost v skladu s tehnično specifikacijo CEN/TS 14793. Zmožnost dokazovanja enakovrednosti mora uradno priznati nacionalni akreditacijski organ ali zakonodaja.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST-TS CEN/TS 16429:2013
01-april-2013
(PLVLMHQHSUHPLþQLKYLURY9]RUþHQMHLQGRORþHYDQMHYRGLNRYHJDNORULGDY
RGYRGQLNLKLQRGYRGQLNLKY]UDN,QIUDUGHþDDQDOL]QDWHKQLND
Stationary source emissions - Sampling and determination of hydrogen chloride content
in ducts and stacks - Infrared analytical technique
Emissionen aus stationären Quellen - Probenahme und Bestimmung von
Chlorwasserstoff in Abgaskanälen und -kaminen - Infrarotverfahren
Émissions de sources fixes - Prélèvement et détermination du chlorure d'hydrogène
dans les conduits et les cheminées - Technique analytique infrarouge
Ta slovenski standard je istoveten z: CEN/TS 16429:2013
ICS:
13.040.40 (PLVLMHQHSUHPLþQLKYLURY Stationary source emissions
SIST-TS CEN/TS 16429:2013 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 16429:2013
TECHNICAL SPECIFICATION
CEN/TS 16429
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
March 2013
ICS 13.040.40
English Version
Stationary source emissions - Sampling and determination of
hydrogen chloride content in ducts and stacks - Infrared
analytical technique
Émissions de sources fixes - Prélèvement et détermination Emissionen aus stationären Quellen - Probenahme und
du chlorure d'hydrogène dans les conduits et les Bestimmung von Chlorwasserstoff in Abgaskanälen und -
cheminées - Technique analytique infrarouge kaminen - Infrarotverfahren
This Technical Specification (CEN/TS) was approved by CEN on 18 September 2012 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
Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2013 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 16429:2013: 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 .8
4.1 General .8
4.2 Measuring principle .8
5 Sampling system .8
5.1 General .8
5.2 Sampling probe .9
5.3 Filter .9
5.4 Sampling line .9
5.5 Conditioning system .9
5.6 Sample pump . 10
5.7 Secondary filter . 10
5.8 Flow controller and flow meter . 10
6 Analyser equipment . 10
6.1 General . 10
6.2 Pressure and temperature effects. 10
6.3 Sampling pump for the analyser . 11
6.4 Interferences due to infrared absorbing gases . 11
7 Determination of the characteristics of the method: analyser, sampling and conditioning
line . 11
7.1 General . 11
7.2 Relevant performance characteristics of the method and performance criteria . 11
7.3 Establishment of the uncertainty budget . 12
8 Field operation . 13
8.1 Measurement plan and sampling strategy . 13
8.2 Setting of the analyser on site . 14
9 Ongoing quality control . 15
9.1 Introduction . 15
9.2 Frequency of checks . 15
10 Expression of results . 16
11 Measurement report . 17
Annex A (informative) Examples of schematics of non-dispersive infrared spectrometer. 18
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Annex B (informative) Example of assessment of compliance of non-dispersive infrared method
for HCl with requirements on emission measurements . 20
Annex C (informative) Procedure for correction of data from drift effect . 31
Bibliography . 32
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Foreword
This document (CEN/TS 16429:2013) 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.
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 an automatic method for determination of the mass concentration of
hydrogen chloride (HCl) in ducts and stacks emitting to atmosphere. It describes the infrared analytical
technique, including the sampling and gas conditioning system. The method should fulfil the performance
characteristics requirements of this Technical Specification and the expanded uncertainty is less than 20 %
relative at the daily Emission Limit Value (ELV).
In order to use an alternative method to this method, it is necessary to demonstrate equivalence according to
the Technical Specification CEN/TS 14793. It is necessary that the capability to demonstrate equivalence is
officially recognised by the national accreditation body or law.
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 15267-3:2007, 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 14956:2002, Air quality — Evaluation of the suitability of a measurement procedure by comparison
with a required measurement uncertainty (ISO 14956:2002)
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
adjustment of a measuring system
set of operations carried out on a measuring system so that it provides prescribed indications corresponding
to given values of a quantity to be measured
[SOURCE: VIM 3.11]
3.2
ambient temperature
temperature of the air around the measuring system
3.3
drift
difference between two zero (zero drift) or span readings (span drift) at the beginning and at the end of a
measuring period
3.4
emission limit value
ELV
emission limit value according to EU Directives on the basis of 30 min, one hour or one day
3.5
influence quantity
quantity that, in a direct measurement, does not affect the quantity that is actually measured, but affects the
measurement result
[SOURCE: VIM 2.52, modified]
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EXAMPLES
− Ambient temperature;
− atmospheric pressure;
− presence of interfering gases in the flue gas matrix;
− pressure of the gas sample.
3.6
interference
negative or positive effect upon the response of the measuring system, due to a component of the sample that
is not the measurand
3.7
lack of fit
systematic deviation within the range of application between the measurement result obtained by applying the
calibration function to the observed response of the measuring system measuring test gases and the
corresponding accepted value of such test gases
Note 1 to entry: Lack of fit may be a function of the measurement result.
Note 2 to entry: The expression “lack of fit” is often replaced in everyday language by “linearity” or “deviation from
linearity”.
3.8
measurand
quantity intended to be measured
[SOURCE: VIM 2.3]
3.9
measuring system
complete set of measuring instruments and other equipment assembled to carry out specified measurements
[SOURCE: VIM 3.2, modified]
3.10
performance characteristic
one of the quantities (described by values, tolerances, range…) assigned to equipment in order to define its
performance
3.11
repeatability in the laboratory
closeness of the agreement between the results of successive measurements of the same measurand carried
out under the same conditions of measurement
Note 1 to entry: Repeatability conditions include:
− the same measurement procedure;
− the same laboratory;
− the same measuring system, used under the same conditions;
− the same location;
− repetition over a short period of time.
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Note 2 to entry: Repeatability may be expressed quantitatively in terms of the dispersion characteristics of the results.
Note 3 to entry: In this Technical Specification, the repeatability is expressed as a value with a level of confidence of
95 %.
[SOURCE: VIM 2.20, modified]
3.12
residence time in the measuring system
time period for the sampled gas to be transported from the inlet of the probe to the inlet of the measurement
cell
3.13
response time
duration between the instant when an input quantity value of a measuring instrument or measuring system is
subjected to an abrupt change between two specified constant quantity values and the instant when a
corresponding indication settles within specified limits around its final steady value
Note 1 to entry: By convention time taken for the output signal to pass from 0 % to 90 % of the final change.
[SOURCE: VIM 4.23, modified]
3.14
sampling plane
plane normal to the centreline of the duct at the sampling position
[SOURCE: EN 13284-1:2001, 3.8]
3.15
sampling point
specific position on a sampling line at which a sample is extracted
[SOURCE: EN 13284-1:2001, 3.10]
3.16
span gas
test gas used to adjust and check a specific point on the response line of the measuring system
Note 1 to entry: This concentration is often chosen around 80 % of the upper limit of the range or around the emission
limit value.
3.17
uncertainty
parameter associated with the result of a measurement, that characterises the dispersion of the values that
could reasonably be attributed to the measurand
3.17.1
standard uncertainty u
uncertainty of the result of a measurement expressed as a standard deviation u
3.17.2
expanded uncertainty U
quantity defining a level of confidence about the result of a measurement that may be expected to encompass
a specific fraction of the distribution of values that could reasonably be attributed to a measurand
U = k . u
Note 1 to entry: In this Technical Specification, the expanded uncertainty is calculated with a coverage factor of k = 2n,
and with a level of confidence of 95 %.
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3.17.3
combined uncertainty u
c
standard uncertainty u attached to the measurement result calculated by combination of several standard
c
uncertainties according to GUM
3.18
uncertainty budget
calculation table combining all the sources of uncertainty according to EN ISO 14956 or ENV 13005 in order
to calculate the expanded uncertainty of the method at a specified value
4 Principle
4.1 General
This Technical Specification describes a method for the determination of the mass concentration of hydrogen
chloride (HCl) in ducts and stacks emitting to atmosphere by means of an automatic analyser using the
infrared absorption principle. The specific components and requirements for the sampling system and the
infrared analyser are described in Clause 6. A number of performance characteristics with associated
minimum performance criteria and an expanded uncertainty of the method are given. Requirements and
recommendations for quality assurance and quality control are given for measurements in the field
(see Table 1 in 7.3).
4.2 Measuring principle
The HCl concentration is measured with an infrared absorption method. The attenuation of infrared light
passing through a sample cell is a measure of the concentration of HCl in the cell, according to the Lambert-
Beer law. Not only HCl but also most hetero-atomic molecules absorb infrared light, in particular water and
CO have broad bands that can interfere with the measurement of HCl. Different technical solutions have
2
been developed to suppress cross-sensitivity, instability and drift in order to design automatic monitoring
systems with acceptable properties. For instance: Gas Filter Correlation, Tunable Diode Laser (TDL) and
Fourier Transform Infrared Spectroscopy (FTIR).
Special attention is paid to infrared light absorbing gases such as water vapour, carbon dioxide, nitrous oxide,
nitrogen dioxide and also hydrocarbons for some special applications.
Infrared analysers are part of extractive or in-situ systems. Most of them are combined with an extractive
sampling system and a gas conditioning system. A representative sample of gas is taken from the stack with a
sampling probe and conveyed to the analyser through the sampling line and gas conditioning system. The
values from the analyser are recorded and/or stored by means of electronic data processing.
The concentration of HCl is measured in volume/volume units (if the analyser is calibrated using a
volume/volume standard). The final results for reporting are expressed in milligrams per cubic meter using
standard conversion factors (see Clause 10).
5 Sampling system
5.1 General
A representative volume (see 8.2.1) is extracted from the flue gas for a fixed period of time at a controlled flow
rate. A filter removes the dust in the sampled volume before the sample is conditioned and passes to the
analyser. Three different sampling and conditioning configurations can be used in order to avoid uncontrolled
water vapour condensation in the measuring system. These configurations are:
configuration 1: removal of water vapour through elimination using a permeation drier;
configuration 2: maintaining the temperature of the sampling line up to the heated analyser;
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configuration 3: for in situ measurements.
Conditions and layout of the sampling equipment contribute to the expanded uncertainty. In order to minimise
this contribution to the expanded uncertainty of the method, performance criteria for the sampling equipment
and sampling conditions are given in 5.2 and 7.2.
5.2 Sampling probe
In order to access the representative sampling point(s) of the sampling plane, probes of different lengths and
inner diameters may be used. The design and configuration of the probe used shall ensure the residence time
of the sample gas within the probe is minimised in order to reduce the response time of the measuring
system.
The procedure described in 8.1 shall be used when a lack of homogeneity in the flue gas is suspected.
5.3 Filter
The filter shall be made of an inert material (e.g. ceramic with an appropriate pore size). The particle filter shall
be changed or cleaned periodically depending on the dust loading at the sampling site.
Overloading of the particle filter may increase the pressure drop in the sampling line.
5.4 Sampling line
The sampling line shall be heated up to the conditioning system, where required. It shall be made of a suitable
corrosion resistant material (e.g. borosilicate glass, ceramic or titanium could be used; PTFE is suitable for
flue gas temperatures lower than 200 °C).
5.5 Conditioning system
5.5.1 Permeation drier (configuration 1)
It is important that all parts of the sampling equipment upstream of the analyser are made of materials that do
not react with or absorb HCl. The temperature of its components coming into contact with the gas shall be
maintained, upstream the permeation system, at a sufficiently high temperature (between 180 °C and 200 °C)
to prevent salt formation and condensation in the sampling equipment (in the presence of water vapour
(beyond in 15 %) and ammonia (few ppm), risk occurs to have salt even at temperatures of 165 °C -170 °C).
The permeation drier is used before the gas enters the analyser in order to separate water vapour from the
flue gas. A dew-point temperature below 4 °C is required at the outlet of the permeation drier.
The concentrations, provided by this sampling configuration, are considered to be given on dry basis.
However, the results may be corrected for the remaining water vapour (refer to the table of Annex A in
EN 14790:2005).
This configuration shall not be used if the flue gas has an ammonia concentration higher than 1 ppm.
5.5.2 Heated line and heated analyser (configuration 2)
It is important that all parts of the sampling equipment upstream of the analyser are made of materials that do
not react with or absorb HCl. The temperature of its components coming into contact with the gas shall be
maintained at a sufficiently high temperature (between 180 °C and 200 °C) to prevent salt formation and
condensation in the sampling equipment (in the presence of water vapour (beyond in 15 %) and ammonia
(few ppm), risk occurs to have salt even at temperatures of 165 °C -170 °C).
If the concentrations are given on wet basis, they shall be corrected so that they are expressed on dry basis.
The correction shall be made from the water vapour concentration measured in the flue gas. The uncertainty
attached to this correction shall be part of the uncertainty budget.
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5.5.3 In situ analysers (configuration 3)
A calibration system, evaluated during the certification process shall be available to determine zero and span
drift for the whole system.
5.6 Sample pump
The sample pump shall be capable of operating to the specified flow requirements of the manufacturer of the
analyser and pressure conditions required for the sample cell. The pump shall be resistant to corrosion. If an
external pump is used it shall be compatible with the requirements of the analyser to which it is connected.
5.7 Secondary filter
The secondary filter is used to separate fine dust, with a pore size less than 5 µm. For example it may be
made of glass-fibre, sintered ceramic, stainless steel or PTFE-fibre.
5.8 Flow controller and flow meter
This apparatus sets the required flow. A corrosion resistant material shall be used. The sample flow rate into
the analyser shall be maintained within the analyser manufacturer’s requirements. A controlled pressure drop
across restrictors is usually employed to maintain flow rate control into the infrared analyser.
NOTE No additional flow controller or flow meter is necessary when they are part of the analyser itself.
6 Analyser equipment
6.1 General
The main parts of the analyser are typically:
source of infrared radiation;
optics to focus the radiation through the measuring cell to the infrared detector;
a way of modulating the infrared beam;
means to select a suitable wavelength or wavelengths to measure the gas;
a measuring cell that the sample gas enters. In some designs there may be a reference cell;
an infrared detector; and
an amplifier and signal processing system to give an electrical output proportional to the HCl
concentration.
The standard of construction and vibration/corrosion resistance shall be suited to industrial environments and
to the composition of the flue gas.
In Annex A, schematic diagrams are given of several different examples of infrared analysers.
6.2 Pressure and temperature effects
The output signal of the analyser is proportional to the number of HCl molecules present in the absorption cell
and depends on the absolute pressure and temperature in the absorption cell. The effects of variations of
pressure and temperature in the absorption cell should be taken into account by the manufacturer to give
results in reference conditions of 273 K and 101,3 kPa.
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6.3 Sampling pump for the analyser
The sampling pump can be separate or part of the analyser. It shall be capable of operating within:
the manufacturer’s specified flow requirements for the analyser; and
the pressure conditions required for the infrared absorption cell.
6.4 Interferences due to infrared absorbing gases
As various gases absorb infrared radiation, interference from these gases can occur when their infrared
absorption bands coincide or overlap the HCl infrared absorption bands. The degree of interference varies
among individual infrared analysers.
The primary interferent is water vapour. However water vapour interference shall be minimised by using
suitable techniques.
If the automated method has been certified the attention shall be focussed on specific interference gases (i.e.
carbon dioxide, hydrocarbons, N O, NO ) which have shown that they have influence on the result.
2 2
Knowledge of the gas composition and the cross sensitivity of the analyser is useful to ensure interference
with the measurement is minimised.
7 Determination of the characteristics of the method: analyser, sampling and
conditioning line
7.1 General
The user of this Technical Specification shall demonstrate that:
the performance characteristics of the method shall be equal or better than the associated performance
criteria given in Table 1 of EN 15267-3:2007; and
the expanded uncertainty of the method calculated by combining values of standard uncertainties
associated with the performance characteristics is less than 20 % at the daily emission limit value, on dry
basis and before correction to the specified value of O .
2
The values of the performance characteristics shall be evaluated by means of a laboratory test and a field
test. An experienced laboratory recognised by the competent authority shall perform the laboratory and field
tests.
It is the responsibility of the user to check the performance characteristics with a periodicity given in Table 2
(Clause 9). These performance characteristics shall be determined using EN 15267-3.
7.2 Relevant performance characteristics of the method and performance criteria
The uncertainty of the measured values by the method is not only influenced by the performance
characteristics of the analyser itself but also by:
the sampling line and conditioning system;
the site specific conditions;
the certified reference material used (e.g. compressed gas in cylinders, certified gas generator).
The performance characteristics of the method shall be evaluated in accordance with EN 15267-3.
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Table 1 of EN 15267-3:2007 gives an overview of the relevant performance characteristics and performance
criteria, which shall be determined during laboratory and field tests according to the relevant CEN procedures,
and indicates values included in the calculation of the expanded uncertainty of the method.
7.3 Establishment of the uncertainty budget
An uncertainty budget shall be established to determine if the analyser and its associated sampling system
fulfil the requirements for a maximum allowable expanded uncertainty of the method.
The method shall have an expanded uncertainty lower than 20 % at the daily emission limit value. This
reference
expanded uncertainty of the method is calculated on a dry basis and before correction to the O
2
concentration. If the concentrations of the automated method are given on a wet basis, a correction to dry
basis shall be carried out. The uncertainty attached to the correction of water vapour content shall be added to
the uncertainty budget. An example of calculation is given in Annex B.
The principle of calculation of the expanded uncertainty of the method is based on the law on propagation of
uncertainty laid down in EN ISO 14956:
determine the sta
...
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