This document specifies a manual method for the determination of the concentration of fluorinated compounds expressed in HF. Two cases are presented:<\/p>\n
first case: the measurand is the concentration of gaseous and bound to particulates fluorides;<\/p>\n<\/li>\n
second case: the measurand is the concentration of gaseous fluorides.<\/p>\n<\/li>\n<\/ul>\n
Three analytical techniques are proposed: ionometry, spectrophotometry and ion-exchange chromatography.<\/p>\n
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.<\/p>\n
This document applies to fluoride concentrations which may vary between 0,1 mg HF\/m3<\/sup> and 10 mg HF\/m3<\/sup>, at standard conditions of pressure and temperature (see NOTE). The limit of quantification of the method is estimated at 0,1 mg\/m3<\/sup> for a sampled volume of 0,1 m3<\/sup>.<\/p>\n Interference may occur for some matrices. Known elements that may lead to interference are mentioned in Annex C.<\/p>\n NOTE The Emission Limit Values (ELV) for HF are expressed in mg\/m3<\/sup>, for dry gases at the standard conditions (T<\/i>std<\/sub> = 273 K and P<\/i>std<\/sub> = 101,3 kPa).<\/p>\n<\/blockquote>\n Stationary source emissions. Determination of mass concentration of fluorinated compounds expressed as HF. Standard reference method<\/b><\/p>\n\n
PDF Catalog<\/h4>\n
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\n PDF Pages<\/th>\n PDF Title<\/th>\n<\/tr>\n \n 2<\/td>\n undefined <\/td>\n<\/tr>\n \n 8<\/td>\n 1 Scope
2 Normative references
3 Terms and definitions <\/td>\n<\/tr>\n\n 14<\/td>\n 4 Symbols and abbreviations
4.1 Symbols <\/td>\n<\/tr>\n\n 16<\/td>\n 4.2 Abbreviations
5 Measuring principle
5.1 General
5.2 Measuring principle <\/td>\n<\/tr>\n\n 17<\/td>\n 6 Sampling equipment
6.1 General
6.2 Sampling line with side stream (first case) <\/td>\n<\/tr>\n\n 18<\/td>\n 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 <\/td>\n<\/tr>\n\n 19<\/td>\n 6.8 Absorbers
6.9 Sample gas pump <\/td>\n<\/tr>\n\n 20<\/td>\n 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 <\/td>\n<\/tr>\n\n 21<\/td>\n 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 <\/td>\n<\/tr>\n\n 22<\/td>\n 7.4 Assembling the equipment
7.5 Field blank
7.6 Heating of the sampling line
7.7 Leak test <\/td>\n<\/tr>\n\n 23<\/td>\n 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 <\/td>\n<\/tr>\n\n 24<\/td>\n 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 <\/td>\n<\/tr>\n\n 25<\/td>\n 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 <\/td>\n<\/tr>\n\n 26<\/td>\n 9.2.2 Sampling procedure
9.2.3 Analysis procedure
9.2.3.1 Sources of uncertainty <\/td>\n<\/tr>\n\n 27<\/td>\n 9.2.4 Performance criterion of analysis <\/td>\n<\/tr>\n \n 28<\/td>\n 9.3 Establishment of the uncertainty budget <\/td>\n<\/tr>\n \n 29<\/td>\n 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) <\/td>\n<\/tr>\n\n 30<\/td>\n 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 <\/td>\n<\/tr>\n\n 31<\/td>\n 11 Test report <\/td>\n<\/tr>\n \n 32<\/td>\n Annex A (informative)Types of sampling devices <\/td>\n<\/tr>\n \n 33<\/td>\n 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 <\/td>\n<\/tr>\n\n 34<\/td>\n 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 <\/td>\n<\/tr>\n\n 35<\/td>\n B.4.4 Operating procedure <\/td>\n<\/tr>\n \n 36<\/td>\n 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 <\/td>\n<\/tr>\n\n 37<\/td>\n 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 <\/td>\n<\/tr>\n\n 38<\/td>\n 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 <\/td>\n<\/tr>\n\n 39<\/td>\n C.3.4.1 Ammonium acetate NH4(CH3COO)
C.3.4.2 Sodium acetate Na(CH3COO)\u00b73H2O
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\u00b0 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 \u00b0C 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) <\/td>\n<\/tr>\n\n 40<\/td>\n 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 <\/td>\n<\/tr>\n\n 41<\/td>\n 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 \u00b0C
C.4.4.2 Ultra-pure water with conductivity < 0,1 \u03bcS\/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 <\/td>\n<\/tr>\n\n 42<\/td>\n C.5 Equipment
C.5.1 Ion chromatography system (see EN ISO 103041) <\/td>\n<\/tr>\n\n 43<\/td>\n C.5.2 Laboratory equipment
C.5.3 Quality criteria for separation column
C.6 Operating procedure <\/td>\n<\/tr>\n\n 44<\/td>\n C.7 Expression of the results <\/td>\n<\/tr>\n \n 45<\/td>\n Annex D (informative)Example of evaluation of compliance of the reference method for HF with emission measurement requirements \u2013 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 <\/td>\n<\/tr>\n\n 46<\/td>\n D.2 Site specific conditions <\/td>\n<\/tr>\n \n 47<\/td>\n D.3 Performance characteristics of the method <\/td>\n<\/tr>\n \n 49<\/td>\n D.4 Calculation of standard uncertainty of the measured concentration
D.4.1 Calculation of total HF concentration <\/td>\n<\/tr>\n\n 51<\/td>\n D.4.2 Model equation and application of the rule of propagation <\/td>\n<\/tr>\n \n 54<\/td>\n D.4.3 Results of standard uncertainty calculations <\/td>\n<\/tr>\n \n 57<\/td>\n 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 <\/td>\n<\/tr>\n\n 58<\/td>\n E.2 Specific conditions in the field
E.3 Performance characteristics of the method <\/td>\n<\/tr>\n\n 59<\/td>\n E.4 Calculation of standard uncertainty of concentration measured
E.4.1 Model equation and application of rule of uncertainty propagation <\/td>\n<\/tr>\n\n 61<\/td>\n E.4.2 Results of the standard uncertainties calculations <\/td>\n<\/tr>\n \n 62<\/td>\n 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 <\/td>\n<\/tr>\n\n 64<\/td>\n Annex F (normative)Determination of water vapour concentration for water saturated gas, at pstd = 101,325 kPa <\/td>\n<\/tr>\n \n 68<\/td>\n 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 <\/td>\n<\/tr>\n\n 70<\/td>\n G.2 Uncertainty associated with a concentration expressed at an oxygen reference concentration <\/td>\n<\/tr>\n<\/table>\n","protected":false},"excerpt":{"rendered":" \n\n
\n Published By<\/td>\n Publication Date<\/td>\n Number of Pages<\/td>\n<\/tr>\n \n BSI<\/b><\/a><\/td>\n 2020<\/td>\n 74<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n","protected":false},"featured_media":422053,"template":"","meta":{"rank_math_lock_modified_date":false,"ep_exclude_from_search":false},"product_cat":[206,2641],"product_tag":[],"class_list":{"0":"post-422042","1":"product","2":"type-product","3":"status-publish","4":"has-post-thumbnail","6":"product_cat-13-040-40","7":"product_cat-bsi","9":"first","10":"instock","11":"sold-individually","12":"shipping-taxable","13":"purchasable","14":"product-type-simple"},"_links":{"self":[{"href":"https:\/\/pdfstandards.shop\/wp-json\/wp\/v2\/product\/422042","targetHints":{"allow":["GET"]}}],"collection":[{"href":"https:\/\/pdfstandards.shop\/wp-json\/wp\/v2\/product"}],"about":[{"href":"https:\/\/pdfstandards.shop\/wp-json\/wp\/v2\/types\/product"}],"wp:featuredmedia":[{"embeddable":true,"href":"https:\/\/pdfstandards.shop\/wp-json\/wp\/v2\/media\/422053"}],"wp:attachment":[{"href":"https:\/\/pdfstandards.shop\/wp-json\/wp\/v2\/media?parent=422042"}],"wp:term":[{"taxonomy":"product_cat","embeddable":true,"href":"https:\/\/pdfstandards.shop\/wp-json\/wp\/v2\/product_cat?post=422042"},{"taxonomy":"product_tag","embeddable":true,"href":"https:\/\/pdfstandards.shop\/wp-json\/wp\/v2\/product_tag?post=422042"}],"curies":[{"name":"wp","href":"https:\/\/api.w.org\/{rel}","templated":true}]}}