kSIST-TS FprCEN/TS 17340:2020

SLOVENSKI STANDARD
oSIST prEN 17340:2018
01-december-2018
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Stationary source emissions - Determination of mass concentration of fluorinated
compounds expressed as HF - Standard reference method
Emissionen aus stationären Quellen - Bestimmung des Massenkonzentration von
gasförmigen Fluoriden, angegeben als HF - Standardreferenzverfahren

Emissions de sources fixes - Détermination de la concentration massique en composés

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

Emissions de sources fixes - Détermination de la Emissionen aus stationären Quellen - Bestimmung des

concentration massique en composés fluorés exprimée Massenkonzentration von gasförmigen Fluoriden,

This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee

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

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,

Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are

Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without

© 2018 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 17340:2018 E

European foreword ....................................................................................................................................................... 6

1 Scope .................................................................................................................................................................... 7

2 Normative references .................................................................................................................................... 7

3 Terms and definitions ................................................................................................................................... 8

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

5 Measuring principle .................................................................................................................................... 15

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

5.2 Measuring principle .................................................................................................................................... 15

6 Sampling equipment ................................................................................................................................... 16

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

6.1.1 Introduction ................................................................................................................................................... 16

6.1.2 Sampling line with side stream (first case) ........................................................................................ 16

6.1.3 Sampling line without side stream (second case) ............................................................................ 17

6.2 Sampling probe ............................................................................................................................................. 17

6.3 Filter housing ................................................................................................................................................. 17

6.4 Particle filter .................................................................................................................................................. 17

6.5 Temperature controller ............................................................................................................................. 17

6.6 Absorbers ........................................................................................................................................................ 18

6.7 Sample gas pump .......................................................................................................................................... 18

6.8 Gas volume meter ........................................................................................................................................ 19

7 Field operation .............................................................................................................................................. 19

7.1 Measurement planning .............................................................................................................................. 19

7.2 Sampling strategy......................................................................................................................................... 19

7.2.1 General ............................................................................................................................................................. 19

7.2.2 Measurement section and measurement plane ................................................................................ 19

7.2.3 Minimum number and location of measurement points ............................................................... 20

7.2.4 Sampling time and volume sampled ..................................................................................................... 20

7.2.5 Measurement ports and working platform ........................................................................................ 20

7.3 Preparation of the glassware and the absorption solution .......................................................... 20

7.4 Assembling the equipment ....................................................................................................................... 21

7.5 Field blank ...................................................................................................................................................... 21

7.6 Heating of the sampling line ..................................................................................................................... 21

7.7 Leak test........................................................................................................................................................... 21

7.8 Performing sampling .................................................................................................................................. 22

7.8.1 Introduction of the sampling probe in the duct ................................................................................ 22

7.8.2 Sampling .......................................................................................................................................................... 22

7.8.3 Rinsing of the sampling system and preparation of the samples ............................................... 23

8 Analysis ............................................................................................................................................................ 23

8.1 General ............................................................................................................................................................. 23

8.2 Preparing samples of washing bottles.................................................................................................. 23

8.3 Methods for treatment of dust collected in the probe and on the filter ................................... 24

Figure 1 ........................................................................................................................................................................... 24

8.4 Analysis ............................................................................................................................................................ 24

9 Determination of the characteristics of the method: sampling and analysis ......................... 24

9.1 General ............................................................................................................................................................. 24

9.2 Performance characteristics for the method and applicable performance criteria ............ 25

9.2.1 General ............................................................................................................................................................. 25

9.2.2 Sampling procedure .................................................................................................................................... 25

9.2.3 Analysis procedure - Sources of uncertainty ...................................................................................... 26

9.2.4 Performance criterion of analysis .......................................................................................................... 27

9.3 Establishment of the uncertainty budget ............................................................................................. 27

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

10.1 Volume of dry sampled gas ....................................................................................................................... 28

10.1.1 General ............................................................................................................................................................. 28

10.1.2 For the main line (particulate Fluorine) .............................................................................................. 28

10.1.3 For the secondary line (gaseous Fluorine) .......................................................................................... 28

10.2 Calculation of HF concentration on dry gas basis ............................................................................. 29

10.3 Expression of results on wet gas basis under standard conditions ........................................... 29

10.4 Expression of results with respect to a reference CO content .................................................... 30

10.5 Expression of results with respect to a reference O content ....................................................... 30

11 Test report ...................................................................................................................................................... 31

Annex A (informative) Type of sampling device ............................................................................................ 32

Annex B (normative) Treatment of filters method ........................................................................................ 33

B.1 Filter treatment with sodium carbonate .............................................................................................. 33

B.2 Modus operandi in case of presence of elements sequestering fluorides ............................... 33

B.3 Alkaline attack ............................................................................................................................................... 33

B.4 Pyrohydrolysis ............................................................................................................................................... 33

B.4.1 Principle ........................................................................................................................................................... 33

B.4.2 Reagents and solutions ............................................................................................................................... 34

B.4.3 Equipment ....................................................................................................................................................... 34

B.4.4 Operating procedure ................................................................................................................................... 35

Annex C (normative) Description of the three analytical techniques for the determination

of HF ................................................................................................................................................................... 36

C.1 Matrix interferences .................................................................................................................................... 36

C.2 Ionometry ........................................................................................................................................................ 36

C.2.1 Principle ........................................................................................................................................................... 36

C.2.2 Scope ................................................................................................................................................................. 36

C.2.3 Reagents ........................................................................................................................................................... 36

C.2.4 Equipment ....................................................................................................................................................... 37

C.2.5 Sampling .......................................................................................................................................................... 37

C.2.6 Operating procedure ................................................................................................................................... 37

C.2.6.1 Calibration ....................................................................................................................................................... 37

C.2.6.2 Determination................................................................................................................................................ 38

C.2.7 Expression of the results ........................................................................................................................... 38

C.3 Spectrophotometry ..................................................................................................................................... 38

C.3.1 Principle .......................................................................................................................................................... 38

C.3.2 Interferents .................................................................................................................................................... 38

C.3.3 Scope ................................................................................................................................................................. 38

C.3.4 Reagents and products ............................................................................................................................... 38

C.3.5 Equipment ...................................................................................................................................................... 40

C.3.6 Operating procedure .................................................................................................................................. 40

C.3.6.1 Blank test ........................................................................................................................................................ 40

C.3.6.2 Measurement ................................................................................................................................................. 40

C.3.6.3 Expression of the results ........................................................................................................................... 40

C.4 Ion chromatography ................................................................................................................................... 41

C.4.1 Principle .......................................................................................................................................................... 41

C.4.2 Interferences ................................................................................................................................................. 41

C.4.3 Limit of detection ......................................................................................................................................... 41

C.4.4 Reagents and solutions .............................................................................................................................. 41

C.5 Equipment ...................................................................................................................................................... 42

C.5.1 Ion chromatography system (see standard EN ISO 10304-1): ..................................................... 42

C.5.2 Laboratory equipment ............................................................................................................................... 43

C.5.3 Quality criteria for separation column ................................................................................................ 43

C.6 Operating procedure .................................................................................................................................. 44

C.7 Expression of the results ........................................................................................................................... 44

Annex D (informative) Example of evaluation of compliance of the reference method for HF

concentration of hydrofluoric acid and gaseous and bound to particulates fluorides ....... 45

D.1 Uncertainty estimation process .............................................................................................................. 45

D.1.1 General ............................................................................................................................................................. 45

D.1.2 Determination of the model equation .................................................................................................. 45

D.1.3 Quantification of uncertainty components ......................................................................................... 45

D.1.4 Calculation of the combined uncertainty ............................................................................................ 45

D.2 Site specific conditions ............................................................................................................................... 46

D.3 Performance characteristics of the method ....................................................................................... 46

D.4 Calculation of standard uncertainty of the measured concentration ....................................... 49

D.4.1 Calculation of total HF concentration ................................................................................................... 49

D.4.2 Model equation and application of the rule of propagation ......................................................... 51

D.4.3 Results of standard uncertainty calculations .................................................................................... 54

Annex E (informative) Example of evaluation of compliance of the reference method for HF

concentration of hydrofluoric acid and gaseous fluorides ............................................................ 57

E.1 Uncertainty estimation process .............................................................................................................. 57

E.1.1 General ............................................................................................................................................................. 57

E.1.2 Determination of the model equation ................................................................................................... 57

E.1.3 Quantification of uncertainty components ......................................................................................... 57

E.1.4 Calculation of the combined uncertainty ............................................................................................. 57

E.2 Specific conditions in the field ................................................................................................................. 58

E.3 Performance characteristics of the method........................................................................................ 59

E.4 Calculation of standard uncertainty of concentration measured ............................................... 60

E.4.1 Model equation and application of rule of uncertainty propagation ........................................ 60

E.4.2 Results of the standard uncertainties calculations .......................................................................... 62

Relative standard uncertainty ............................................................................................................................... 62

E.4.3 Estimation of the combined uncertainty .............................................................................................. 63

E.5 Calculation of the overall (or expanded) uncertainty ..................................................................... 63

reference concentration ............................................................................................................................. 63

Annex F (normative) Determination of water vapour concentration for water saturated

gas, at p = 101,325 kPa ......................................................................................................................... 65

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

expressed on dry gas and at an oxygen reference concentration ............................................... 69

G.1 Uncertainty associated with a concentration expressed on dry gas .......................................... 69

concentration ................................................................................................................................................. 71

Bibliography ................................................................................................................................................................. 74

This document (prEN 17340:2018) has been prepared by Technical Committee CEN/TC 264 “Air

This document specifies a manual method for the determination of the concentration of fluorinated

— first case: the measurand is the concentration of hydrofluoric acid and gaseous and bound to

— second case: the measurand is the concentration of hydrofluoric acid and gaseous fluorides.

Three analytical techniques are proposed: ionometry, spectrophotometry and ion-exchange

This document specifies the performance characteristics to be determined and the performance criteria

to be fulfilled when it is used as the Standard Reference Method (SRM) for periodic monitoring and for

calibration or control of Automated Measuring Systems (AMS) permanently installed on a stack, for

This document applies to more or less dust-laden flue gases whose HF concentration may vary between

0,1 mg/m and 10 mg/m , at standard conditions of pressure and temperature (see NOTE). The

quantification limit of the method is estimated at 0,1 mg/m for a sampled volume of 0,1 m .

Interference may occur for some matrices. Known elements that may lead to interference are mentioned

NOTE The Emission Limit Values (ELV) are expressed in mg HF/m , for dry gases at the standard conditions:

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 1911, Determination of mass concentration of gaseous chlorides expressed as HCl — Standard reference

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

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

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

EN 13284-1, Stationary source emissions - Determination of low range mass concentration of dust - Part 1:

EN ISO 10304-1, Water quality - Determination of dissolved anions by liquid chromatography of ions - Part

1: Determination of bromide, chloride, fluoride, nitrate, nitrite, phosphate and sulfate (ISO 10304-1)

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

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

device in which the compound to be trapped is absorbed into the absorption solution

ratio of quantity of the analyte q collected in the first absorber divided by the quantity of the analyte

measurement method which complies with the criteria given by this European Standard with respect to

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

closeness of the agreement between the results of successive measurements of the same measurand