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BSI PD CEN/TS 17340:2020

BSI PD CEN/TS 17340:2020

$215.11

Stationary source emissions. Determination of mass concentration of fluorinated compounds expressed as HF. Standard reference method

Published By Publication Date Number of Pages
BSI 2020 74
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This document specifies a manual method for the determination of the concentration of fluorinated compounds expressed in HF. Two cases are presented:

  • first case: the measurand is the concentration of gaseous and bound to particulates fluorides;

  • second case: the measurand is the concentration of gaseous fluorides.

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

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 regulatory or other purposes.

This document applies to fluoride concentrations which may vary between 0,1 mg HF/m3 and 10 mg HF/m3, at standard conditions of pressure and temperature (see NOTE). The limit of quantification of the method is estimated at 0,1 mg/m3 for a sampled volume of 0,1 m3.

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

NOTE The Emission Limit Values (ELV) for HF are expressed in mg/m3, for dry gases at the standard conditions (Tstd = 273 K and Pstd = 101,3 kPa).

PDF Catalog

PDF Pages PDF Title
2 undefined
8 1 Scope
2 Normative references
3 Terms and definitions
14 4 Symbols and abbreviations
4.1 Symbols
16 4.2 Abbreviations
5 Measuring principle
5.1 General
5.2 Measuring principle
17 6 Sampling equipment
6.1 General
6.2 Sampling line with side stream (first case)
18 6.3 Sampling line without side stream (second case)
6.4 Sampling probe
6.5 Filter housing
6.6 Particle filter
6.7 Temperature controller
19 6.8 Absorbers
6.9 Sample gas pump
20 6.10 Gas volume meter
7 Field operation
7.1 Measurement planning
7.2 Sampling strategy
7.2.1 General
7.2.2 Measurement section and measurement plane
21 7.2.3 Minimum number and location of measurement points
7.2.4 Sampling time and volume sampled
7.2.5 Measurement ports and working platform
7.3 Preparation of the glassware and the absorption solution
22 7.4 Assembling the equipment
7.5 Field blank
7.6 Heating of the sampling line
7.7 Leak test
23 7.8 Performing sampling
7.8.1 Introduction of the sampling probe in the duct
7.8.2 Sampling
7.8.3 Rinsing of the sampling system and preparation of the samples
24 8 Analysis
8.1 General
8.2 Preparing samples of absorbers
8.3 Methods for treatment of dust collected in the probe and on the filter
25 8.4 Analysis
9 Determination of the characteristics of the method: sampling and analysis
9.1 General
9.2 Performance characteristics for the method and applicable performance criteria
9.2.1 General
26 9.2.2 Sampling procedure
9.2.3 Analysis procedure
9.2.3.1 Sources of uncertainty
27 9.2.4 Performance criterion of analysis
28 9.3 Establishment of the uncertainty budget
29 10 Expression of results
10.1 Volume of dry sampled gas
10.1.1 General
10.1.2 For the main line (bound to particulate fluorides)
10.1.3 For the secondary line (gaseous Fluorides)
30 10.2 Calculation of HF concentration on dry gas basis
10.3 Expression of results on wet gas basis under standard conditions
10.4 Expression of results with respect to a reference O2 content
31 11 Test report
32 Annex A (informative)Types of sampling devices
33 Annex B (normative)Treatment of filters method (first case)
B.1 Filter treatment with sodium carbonate
B.2 Modus operandi in case of presence of elements sequestering fluorides
B.3 Alkaline attack
B.4 Pyrohydrolysis
B.4.1 Principle
34 B.4.2 Reagents and solutions
B.4.2.1 Sodium hydroxide solution (NaOH)
B.4.2.2 Vanadium oxide (V2O5)
B.4.2.3 Sodium hydroxide solution (4 g/l) prepared from solution (B.4.2.1)
B.4.3 Equipment
35 B.4.4 Operating procedure
36 Annex C (normative)Description of the three analytical techniques for the determination of HF
C.1 Matrix interferences
C.2 Ionometry
C.2.1 Principle
C.2.2 Scope
C.2.3 Reagents
37 C.2.3.1 Buffer solution
C.2.3.2 Fluoride ion standard stock solution (1 g/l)
C.2.4 Equipment
C.2.5 Sampling
C.2.6 Operating procedure
C.2.6.1 Calibration
38 C.2.6.2 Determination
C.2.7 Expression of the results
C.3 Spectrophotometry
C.3.1 Principle
C.3.2 Interferents
C.3.3 Scope
C.3.4 Reagents and products
39 C.3.4.1 Ammonium acetate NH4(CH3COO)
C.3.4.2 Sodium acetate Na(CH3COO)·3H2O
C.3.4.3 Glacial acetic acid d = 1,05 CH3COOH
C.3.4.4 Lanthanum oxide La2O3
C.3.4.5 Hydrochloric acid (HCI) 2 N
C.3.4.6 Acetone CH3COCH3
C.3.4.7 Ethanol 96° GL CH3CH2OH
C.3.4.8 Alizarin complexone (amino acid-methyl-3-NN Alizarin diacetic: C19H15NO8)
C.3.4.9 Combined lanthanum-alizarin complexone reagent
C.3.4.10 Sodium fluoride dried at 110 °C NaF
C.3.4.11 Phenolphthalein
C.3.4.12 Ammonia NH4OH d = 0,92
C.3.4.13 Ammonium acetate solution (200 g/l)
C.3.4.14 Alcoholic phenolphthalein solution (0,1 %) prepared by dissolving phenolphthalein (C.3.4.11) in ethanol (C.3.4.7)
C.3.4.15 Hydrochloric acid solution approximately 0,1 N
C.3.4.16 Fluoride solution (1 g/l)
40 C.3.4.17 Fluoride solution (5 mg/l)
C.3.5 Equipment
C.3.6 Operating procedure
C.3.6.1 Blank test
C.3.6.2 Measurement
41 C.3.6.3 Expression of the results
C.4 Ion chromatography
C.4.1 Principle
C.4.2 Interferences
C.4.3 Limit of detection
C.4.4 Reagents and solutions
C.4.4.1 Sodium fluoride dried at 110 °C
C.4.4.2 Ultra-pure water with conductivity < 0,1 μS/cm
C.4.4.3 Fluoride solution 1000 mg/l (stock solution) prepared by weighing of 2,23 g of NaF in 1,0 l of water
C.4.4.4 Store the solution and the diluted solutions used for calibration (see C.6) in a plastic container.
C.4.4.5 Eluents
42 C.5 Equipment
C.5.1 Ion chromatography system (see EN ISO 103041)
43 C.5.2 Laboratory equipment
C.5.3 Quality criteria for separation column
C.6 Operating procedure
44 C.7 Expression of the results
45 Annex D (informative)Example of evaluation of compliance of the reference method for HF with emission measurement requirements – First case: the measurand is the concentration of hydrofluoric acid and gaseous and bound to particulates fluorides
D.1 Uncertainty estimation process
D.1.1 General
D.1.2 Determination of the model equation
D.1.3 Quantification of uncertainty components
D.1.4 Calculation of the combined uncertainty
46 D.2 Site specific conditions
47 D.3 Performance characteristics of the method
49 D.4 Calculation of standard uncertainty of the measured concentration
D.4.1 Calculation of total HF concentration
51 D.4.2 Model equation and application of the rule of propagation
54 D.4.3 Results of standard uncertainty calculations
57 Annex E (informative)Example of evaluation of compliance of the reference method for HF with emission measurement requirements – Second case: the measurand is the concentration of hydrofluoric acid and gaseous fluorides
E.1 Uncertainty estimation process
E.1.1 General
E.1.2 Determination of the model equation
E.1.3 Quantification of uncertainty components
E.1.4 Calculation of the combined uncertainty
58 E.2 Specific conditions in the field
E.3 Performance characteristics of the method
59 E.4 Calculation of standard uncertainty of concentration measured
E.4.1 Model equation and application of rule of uncertainty propagation
61 E.4.2 Results of the standard uncertainties calculations
62 E.4.3 Estimation of the combined uncertainty
E.5 Calculation of the overall (or expanded) uncertainty
E.6 Uncertainty associated to the mass concentration of gaseous fluorides at O2 reference concentration
64 Annex F (normative)Determination of water vapour concentration for water saturated gas, at pstd = 101,325 kPa
68 Annex G (informative)Calculation of the uncertainty associated with a concentration expressed on dry gas and at an oxygen reference concentration
G.1 Uncertainty associated with a concentration expressed on dry gas
70 G.2 Uncertainty associated with a concentration expressed at an oxygen reference concentration

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BSI PD CEN/TS 17340:2020
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