Stationary source emissions - Determination of mass concentration of multiple gaseous species - Fourier transform infrared spectroscopy

This Technical Specification describes a method for sampling and determining the concentration of gaseous emissions to atmosphere of multiple species from ducts and stacks by extractive Fourier transform infrared (FTIR) spectroscopy. This method is applicable to periodic monitoring and to the calibration or control of Automated Measuring Systems (AMS) permanently installed on a stack for regulatory or other purposes.

Emissionen aus stationären Quellen - Messung von Emissionen im Abgas mit FTIR-Geräten

Dieses Dokument beschreibt ein Verfahren zur Probenahme und Bestimmung der Konzentration von gasförmigen Emissionen mehrerer Stoffe in die Atmosphäre aus Leitungen und Abgaskanälen mithilfe der extraktiven Fourier-Transform-Infrarot (FTIR)-Spektroskopie.
Dieses Verfahren ist für die wiederkehrende Überwachung und für die Kalibrierung oder Kontrolle von dauerhaft an einem Abgaskanal installierten automatischen Messeinrichtungen (AMS) aufgrund gesetzlicher Vorschriften oder für andere Zwecke anwendbar.

Émissions de sources fixes - Détermination de la concentration en masse de multiples substances gazeuses - Spectroscopie infrarouge à transformée de Fourier

Emisije nepremičnih virov - Določevanje masne koncentracije posameznih plinov v zmesi - Infrardeča spektroskopija s Fourierjevo transformacijo (FTIR)

Ta tehnična specifikacija opisuje metodo za vzorčenje in določevanje koncentracije plinastih emisij v ozračju pri več zvrsteh iz vodov in odvodnikov z infrardečo spektroskopijo s Fourierjevo transformacijo (FTIR). Ta metoda se uporablja za redno spremljanje in umerjanje ali nadzor avtomatskih merilnih sistemov (AMS), ki so trajno nameščeni na odvodnik, in sicer za zakonske ter druge namene.

General Information

Status
Published
Public Enquiry End Date
24-Feb-2019
Publication Date
25-Jun-2019
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
13-Jun-2019
Due Date
18-Aug-2019
Completion Date
26-Jun-2019

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SLOVENSKI STANDARD
SIST-TS CEN/TS 17337:2019
01-september-2019
Emisije nepremičnih virov - Določevanje masne koncentracije posameznih plinov
v zmesi - Infrardeča spektroskopija s Fourierjevo transformacijo (FTIR)

Stationary source emissions - Determination of mass concentration of multiple gaseous

species - Fourier transform infrared spectroscopy
Emissionen aus stationären Quellen - Messung von Emissionen im Abgas mit FTIR-
Geräten

Émissions de sources fixes - Détermination de la concentration en masse de multiples

substances gazeuses - Spectroscopie infrarouge à transformée de Fourier
Ta slovenski standard je istoveten z: CEN/TS 17337:2019
ICS:
13.040.40 Emisije nepremičnih virov Stationary source emissions
SIST-TS CEN/TS 17337:2019 en

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST-TS CEN/TS 17337:2019
CEN/TS 17337
TECHNICAL SPECIFICATION
SPÉCIFICATION TECHNIQUE
June 2019
TECHNISCHE SPEZIFIKATION
ICS 13.040.40
English Version
Stationary source emissions - Determination of mass
concentration of multiple gaseous species - Fourier
transform infrared spectroscopy

Émissions de sources fixes - Détermination de la Emissionen aus stationären Quellen - Messung von

concentration en masse de multiples substances Emissionen im Abgas mit FTIR-Geräten

gazeuses - Spectroscopie infrarouge à transformée de
Fourier

This Technical Specification (CEN/TS) was approved by CEN on 1 April 2019 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, Serbia, 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: Rue de la Science 23, B-1040 Brussels

© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 17337:2019 E

worldwide for CEN national Members.
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Contents Page

European foreword ....................................................................................................................................................... 5

1 Scope .................................................................................................................................................................... 6

2 Normative references .................................................................................................................................... 6

3 Terms and definitions ................................................................................................................................... 6

4 Symbols and abbreviations ...................................................................................................................... 14

4.1 Symbols ............................................................................................................................................................ 14

4.2 Abbreviated terms ....................................................................................................................................... 15

5 Principle .......................................................................................................................................................... 15

5.1 General ............................................................................................................................................................. 15

5.2 Measuring Principle .................................................................................................................................... 15

6 Sampling system ........................................................................................................................................... 16

6.1 General ............................................................................................................................................................. 16

6.2 Apparatus requirements ........................................................................................................................... 16

6.2.1 General ............................................................................................................................................................. 16

6.2.2 Sampling probe ............................................................................................................................................. 16

6.2.3 Filter .................................................................................................................................................................. 16

6.2.4 Sample gas line .............................................................................................................................................. 17

6.2.5 Pump ................................................................................................................................................................. 17

6.2.6 Oxygen sensor (optional) .......................................................................................................................... 17

7 Determination of the performance characteristics of the method ............................................ 17

7.1 Measured components covered by SRM .............................................................................................. 17

7.2 Measured components not covered by SRM ....................................................................................... 18

7.3 Establishment of an uncertainty budget .............................................................................................. 18

8 Field operation .............................................................................................................................................. 18

8.1 Measurement site ......................................................................................................................................... 18

8.2 Measurement points ................................................................................................................................... 18

8.3 Choice of the measuring system ............................................................................................................. 18

8.4 Setting up of the analyser on site ........................................................................................................... 19

8.4.1 General ............................................................................................................................................................. 19

8.4.2 Selection of test gases ................................................................................................................................. 19

8.4.3 Tests at the start of measurement period ........................................................................................... 21

8.4.4 Emission measurements ........................................................................................................................... 23

8.4.5 Tests at the end of the measurement period ..................................................................................... 25

8.4.6 Determining drift across measurement period ................................................................................ 25

9 Ongoing quality control ............................................................................................................................. 25

9.1 Introduction ................................................................................................................................................... 25

9.2 Frequency of checks .................................................................................................................................... 26

9.3 Annual calibration or calibration validation ..................................................................................... 27

9.3.1 General ............................................................................................................................................................. 27

9.3.2 Annual calibration ....................................................................................................................................... 27

9.3.3 Calibration validation ................................................................................................................................. 27

9.4 Annual response time test ........................................................................................................................ 28

9.5 Measurement campaign data storage ................................................................................................... 28

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10 Expression of results ................................................................................................................................... 28

11 Measurement report ................................................................................................................................... 29

Annex A (informative) Sampling with a side stream .................................................................................... 30

Annex B (normative) Detection limit, computational interference and annual tests ...................... 31

B.1 General ............................................................................................................................................................. 31

B.2 Response time ................................................................................................................................................ 31

B.3 Detection limit ............................................................................................................................................... 31

B.3.1 General ............................................................................................................................................................. 31

B.3.2 Approach A ...................................................................................................................................................... 32

B.3.3 Approach B ...................................................................................................................................................... 32

B.4 Computational interferent test for components not covered by SRM ....................................... 32

B.5 Annual lack of fit test ................................................................................................................................... 33

B.5.1 Description of test procedure .................................................................................................................. 33

B.5.2 Establishment of the regression line ..................................................................................................... 33

B.5.3 Calculation of the residuals ....................................................................................................................... 34

B.5.4 Test requirements ........................................................................................................................................ 35

Annex C (informative) Uncertainty determination ....................................................................................... 36

C.1 General ............................................................................................................................................................. 36

C.2 Elements required for the uncertainty determinations ................................................................. 36

C.2.1 Model function ............................................................................................................................................... 36

C.2.2 Determination of uncertainty .................................................................................................................. 36

C.2.3 Combined standard uncertainty ............................................................................................................. 37

C.2.4 Expanded uncertainty ................................................................................................................................. 38

C.2.5 Uncertainty budget template ................................................................................................................... 39

C.3 Example uncertainty budget .................................................................................................................... 39

C.3.1 General ............................................................................................................................................................. 39

C.3.2 Identification of uncertainty sources .................................................................................................... 39

C.3.2.1 General ............................................................................................................................................................. 39

C.3.2.2 Concentration indicated by the analyser ............................................................................................. 40

C.3.2.3 Uncertainty sources with rectangular probability distributions ................................................ 40

C.3.2.4 Cross-sensitivity ............................................................................................................................................ 41

C.3.2.5 Uncertainty sources with normal probability distributions ........................................................ 41

C.3.3 Site specific conditions ............................................................................................................................... 42

C.3.4 Result of example uncertainty calculation .......................................................................................... 42

C.4 Comparison of expanded uncertainty to required measurement uncertainty ...................... 47

Annex D (informative) Selection of test gases for Check Gas approach ................................................. 48

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D.1 General ............................................................................................................................................................. 48

D.2 Example 1 ........................................................................................................................................................ 48

D.3 Example 2 ........................................................................................................................................................ 49

Annex E (informative) Example of correction of data from drift effect ................................................. 54

Annex F (informative) Calculation of the uncertainty associated with a concentration

expressed on dry gas and at an oxygen reference concentration .............................................. 56

F.1 Uncertainty associated with a concentration expressed on dry gas ......................................... 56

F.2 Uncertainty associated with a concentration expressed at a oxygen reference

concentration ................................................................................................................................................ 58

Bibliography ................................................................................................................................................................. 60

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European foreword

This document (CEN/TS 17337:2019) 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 shall not be held responsible for identifying any or all such patent rights.

According to the CEN/CENELEC Internal Regulations, the national standards organisations 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, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,

Turkey and the United Kingdom.
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1 Scope

This document describes a method for sampling and determining the concentration of gaseous emissions

to atmosphere of multiple species from ducts and stacks by extractive Fourier transform infrared (FTIR)

spectroscopy.

This method is applicable to periodic monitoring and to the calibration or control of automated

measuring systems (AMS) permanently installed on a stack, for regulatory or other purposes.

2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements 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.

EN 14793:2017, Stationary source emissions - Demonstration of equivalence of an alternative method with

a reference method

EN 15259:2007, Air quality - Measurement of stationary source emissions - Requirements for measurement

sections and sites and for the measurement objective, plan and report

EN 15267-4:2017, Air quality - Certification of automated measuring systems - Part 4: Performance criteria

and test procedures for automated measuring systems for periodic measurements of emissions from

stationary sources

EN ISO 14956, Air quality - Evaluation of the suitability of a measurement procedure by comparison with a

required measurement uncertainty (ISO 14956)

ISO/IEC Guide 98-3:2008, Uncertainty of measurement — Part 3: Guide to the expression of uncertainty in

measurement (GUM:1995)
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— IEC Electropedia: available at http://www.electropedia.org/
— ISO Online browsing platform: available at http://www.iso.org/obp
3.1
FTIR spectrometer

interferometer that uses infrared wavelengths of the electromagnetic spectrum for measurements and

normally includes a sample cell and detector

Note 1 to entry: The interferometer records an interferogram which represents the detection systems response

as a function of time. The Fourier-transform function is applied to produce optical intensity as a function of

frequency or wavelength.
3.2
sample cell

part of the FTIR instrument where the infrared beam is transmitted through the sample

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3.3
standard reference method
SRM
reference method prescribed by European or national legislation
[SOURCE: EN 15259:2007]
3.4
reference method

measurement method taken as a reference by convention, which gives the accepted reference value of

the measurand
Note 1 to entry: A reference method is fully described
Note 2 to entry: A reference method can be a manual or an automated method

Note 3 to entry: Alternative methods can be used if equivalence to the reference method has been demonstrated

[SOURCE: EN 15259:2007]
3.5
alternative method

measurement method which complies with the criteria given by EN 14793 with respect to the reference

method

Note 1 to entry: An alternative method can consist of a simplification of the reference method.

[SOURCE: EN 14793:2017]
3.6
measuring system

set of one or more measuring instruments and often other devices, including any reagent and supply,

assembled and adapted to give information used to generate measured quantity values within specified

intervals for quantities of specified kinds
[SOURCE: JCGM 200:2012]
3.7
automated measuring system
AMS

entirety of all measuring instruments and additional devices for obtaining a result of measurement

Note 1 to entry: Apart from the actual measuring device (the analyser), an AMS includes facilities for taking

samples (e.g. probe, sample gas lines, flow meters and regulator, delivery pump) and for sample conditioning (e.g.

dust filter, pre-separator for interferents, cooler, converter). This definition also includes testing and adjusting

devices that are required for functional checks and, if applicable, for commissioning.

Note 2 to entry: The term “automated measuring system” (AMS) is typically used in Europe. The term

“continuous emission monitoring system” (CEMS) is also typically used in the UK and USA.

[SOURCE: EN 15267-4:2017]
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3.8
portable automated measuring system
P-AMS

automated measuring system which is in a condition or application to be moved from one to another

measurement site to obtain measurement results for a short measurement period
Note 1 to entry: The measurement period is typically 8 h for a day.

Note 2 to entry: The P-AMS can be configured at the measurement site for the special application but can be also

set-up in a van or mobile container. The probe and the sample gas lines are installed often just before the

measurement task is started.
[SOURCE: EN 15267-4:2017]
3.9
calibration

set of operations that establish, under specified conditions, the relationship between values of quantities

indicated by a measuring method or measuring system, and the corresponding values given by the

applicable reference

Note 1 to entry: In case of automated measuring system (AMS) permanently installed on a stack the applicable

reference is the standard reference method (SRM) used to establish the calibration function of the AMS.

Note 2 to entry: Calibration should not be confused with adjustment of a measuring system.

[SOURCE: EN 15058:2017]
3.10
adjustment

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

Note 1 to entry: The adjustment can be made directly on the instrument or using a suitable calculation procedure.

[SOURCE: EN 15058:2017]
3.11
span gas

test gas used to adjust and check a specific point on the response line of the measuring system

[SOURCE: EN 15058:2017]
3.12
measurand
particular quantity subject to measurement

Note 1 to entry: The measurand is a quantifiable property of the waste gas under test, for example mass

concentration of a measured component, temperature, velocity, mass flow, oxygen content and water vapour

content.
[SOURCE: EN 15259:2007]
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3.13
interference

negative or positive effect upon the response of the measuring system, due to a component of the sample

that is not the measurand
[SOURCE: EN 15058:2017]
3.14
influence quantity

quantity that is not the measurand but that affects the result of the measurement

Note 1 to entry: Influence quantities are e.g. presence of interfering gases, ambient temperature, pressure of the

gas sample.
[SOURCE: EN 15058:2017]
3.15
ambient temperature
temperature of the air around the measuring system
[SOURCE: EN 15058:2017]
3.16
emission limit value
ELV

limit value given in regulations such as EU Directives, ordinances, administrative regulations, permits,

licences, authorisations or consents

Note 1 to entry: ELV can be stated as concentration limits expressed as half-hourly, hourly and daily averaged

values, or mass flow limits expressed as hourly, daily, weekly, monthly or annually aggregated values.

[SOURCE: EN 15058:2017]
3.17
measuring campaign

given by the measurement task described in the measurement plan in accordance with EN 15259

3.18
measuring period
period encompassed by the drift test
3.19
measurement site

place on the waste gas duct in the area of the measurement plane(s) consisting of structures and technical

equipment, for example working platforms, measurement ports, energy supply
Note 1 to entry: Measurement site is also known as sampling site.
[SOURCE: EN 15259:2007]
3.20
measurement plane
plane normal to the centreline of the duct at the sampling position
Note 1 to entry: Measurement plane is also known as sampling plane.
[SOURCE: EN 15259:2007]
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3.21
measurement port

opening in the waste gas duct along the measurement line, through which access to the waste gas is

gained
Note 1 to entry: Measurement port is also known as sampling port or access port.
[SOURCE: EN 15259:2007]
3.22
measurement line

line in the measurement plane along which the measurement points are located, bounded by the inner

duct wall
Note 1 to entry: Measurement line is also known as sampling line.
[SOURCE: EN 15259:2007]
3.23
measurement point

position in the measurement plane at which the sample stream is extracted or the measurement data are

obtained directly
Note 1 to entry: Measurement point is also known as sampling point.
[SOURCE: EN 15259:2007]
3.24
absorbance spectrum
negative logarithm of the transmission spectrum
3.25
transmittance spectrum

ratio of a single channel spectrum where the component(s) is present to a single channel spectrum where

it is not (the background), both spectra being acquired under the same conditions

3.26
background spectrum

single channel spectrum recorded in the absence of component (usually zero gas) used for deriving the

transmission spectrum
3.27
single channel spectrum

response of the FTIR instrument as a function of wavenumber to a sample of either the component(s) or

background
3.28
spectral feature
referring to one or more absorbance peaks in a spectrum
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3.29
resolution

minimum separation that two spectral features can have and still be distinguished from one another

Note 1 to entry: Defined as the reciprocal of the optical path difference of the interferometer.

3.30
analytical window

upper and lower wavenumber range (or set of ranges) between which the measurand is interpreted the

instruments analytical model
3.31
analytical model

algorithm used to interpret a spectrum and output quantitative (or qualitative) information

Note 1 to entry: The analytical model will usually fit (in a least squares sense) reference spectra to a spectrum of

the sample in order to identify which compounds are present and derive concentration data.

3.32
performance characteristic
quantity assigned to the P-AMS in order to define its performance

Note 1 to entry: The values of relevant performance characteristics are determined in the performance testing and

compared to the applicable performance criteria.
[SOURCE: EN 15267-4:2017]
3.33
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 variation of

indication.
[SOURCE: EN 15058:2017]
3.34
drift

difference between two readings of a reference material at the beginning and at the end of a measuring

period
3.35
lack of fit

systematic deviation, within the measurement range, between the accepted value of a reference material

applied to the measuring system and the corresponding result of measurement produced by the

calibrated measuring system

Note 1 to entry: In common language lack of fit is often called “linearity” or “deviation from linearity”. Lack of fit

test is often called “linearity test”.
[SOURCE: EN 15267-4:20
...

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