EN 14791-2005 8093 Stationary source emissions - Determination of mass concentration of sulphur dioxide - Reference method《固定排放源 二氧化硫质量浓度的测定 参照法》.pdf

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1、BRITISH STANDARDBS EN 14791:2005Stationary source emissions Determination of mass concentration of sulphur dioxide Reference methodThe European Standard EN 14791:2005 has the status of a British StandardICS 13.040.40g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g

2、54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58Licensed Copy: Wang Bin, na, Tue Apr 18 03:14:21 BST 2006, Uncontrolled Copy, (c) BSIBS EN 14791:2005This British Standard was published under the authority of the Standards Policy and

3、 Strategy Committee on 16 January 2006 BSI 16 January 2006ISBN 0 580 46978 6National forewordThis British Standard is the official English language version of EN 14791:2005.The UK participation in its preparation was entrusted by Technical Committee EH/2, Air quality, to Subcommittee EH/2/1, Station

4、ary source emissions, which has the responsibility to: A list of organizations represented on this subcommittee can be obtained on request to its secretary.Cross-referencesThe British Standards which implement international or European publications referred to in this document may be found in the BS

5、I Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for i

6、ts correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep UK interests

7、informed; monitor related international and European developments and promulgate them in the UK.Summary of pagesThis document comprises a front cover, an inside front cover, the EN title page, pages 2 to 61 and a back cover.The BSI copyright notice displayed in this document indicates when the docum

8、ent was last issued.Amendments issued since publicationAmd. No. Date CommentsLicensed Copy: Wang Bin, na, Tue Apr 18 03:14:21 BST 2006, Uncontrolled Copy, (c) BSIEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 14791November 2005ICS 13.040.40English VersionStationary source emissions - Determinatio

9、n of massconcentration of sulphur dioxide - Reference methodEmissions de sources fixes - Dtermination de laconcentration massique du dioxide de soufre - Mthode derfrenceEmissionen aus stationren Quellen - Bestimmung derMassenkonzentration von Schwefeldioxid -ReferenzverfahrenThis European Standard w

10、as approved by CEN on 30 September 2005.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such

11、nationalstandards may be obtained on application to the Central Secretariat or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and n

12、otified to the Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherl

13、ands, Norway, Poland, Portugal, Slovakia,Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2005 CEN All rights of exploitation in any form an

14、d by any means reservedworldwide for CEN national Members.Ref. No. EN 14791:2005: ELicensed Copy: Wang Bin, na, Tue Apr 18 03:14:21 BST 2006, Uncontrolled Copy, (c) BSIEN 14791:2005 (E) 2 Contents Page Foreword 5 1 Scope .6 2 Normative references .6 3 Terms, definitions, symbols and abbreviations .6

15、 3.1 Terms and definitions.6 3.2 Symbols.11 3.3 Abbreviations 12 4 Principle.13 4.1 General 13 4.2 Measuring principle 13 5 Reagents13 5.1 General 13 5.2 Hydrogen peroxide .13 5.3 Water13 5.4 Absorption solution, H2O213 5.5 Reagents for chromatographic analysis .14 5.5.1 Eluent solution 14 5.5.2 Sta

16、ndard sulphate stock solution, 10,4x10-3mol/l 24SO 14 5.5.3 Regeneration solution for suppressor 14 5.6 Reagent for Thorin analysis.14 5.6.1 2-propanol CH3CH(OH)CH314 5.6.2 Barium perchlorate, standard volumetric solution, Ba(CIO4)2 = 0,005 mol/l14 5.6.3 Potassium hydroxide, standard volumetric solu

17、tion, KOH = 0,1 mol/l.15 5.6.4 Perchloric acid, standard volumetric solution, HClO4 = 0,1 mol/l.15 5.6.5 Thorin, 4-2-arsonophenyl)-azo-3-hydroxy-2,7 naphthalene-disulfonic acid disodium salt 2 g/l solution.15 6 Sampling equipment.15 6.1 General 15 6.2 Sampling probe.15 6.3 Filter housing 16 6.4 Part

18、icle filter 16 6.5 Temperature controller.16 6.6 Absorbers16 6.6.1 General 16 Licensed Copy: Wang Bin, na, Tue Apr 18 03:14:21 BST 2006, Uncontrolled Copy, (c) BSIEN 14791:2005 (E) 3 6.6.2 Test of absorption efficiency .17 6.7 Sampling pump .17 6.8 Gas volume meter.17 7 Sampling procedure .18 7.1 Ge

19、neral requirements.18 7.2 Preparation and installation of equipment18 7.2.1 Sampling location .18 7.2.2 Sampling point(s)18 7.2.3 Assembling the equipment 19 7.2.4 Heating of the sampling line 19 7.2.5 Leak test 19 7.3 Performing sampling 19 7.3.1 Introduction of the probe in the duct.19 7.3.2 Sampl

20、ing19 7.3.3 Rinsing of the sampling system and preparation of the samples.20 7.4 Measuring series.20 7.5 Field blank .20 7.6 Absorption efficiency .21 8 Analysis equipment 21 8.1 Ion chromatograph .21 8.2 Thorin method.22 8.2.1 General 22 8.2.2 Spectrophotometer (optional)22 8.2.3 Glass optical cuve

21、tte 22 9 Analytical procedure.22 9.1 General 22 9.2 Ion Chromatography method.22 9.2.1 General procedure 22 9.2.2 Interferences .23 9.2.3 Calibration .23 9.3 Thorin Method.24 9.3.1 Pre-treatment of sample solution before analysis for Thorin method24 9.3.2 General procedure 24 9.3.3 Preparation of a

22、chemical blank solution .25 9.3.4 Interferents 25 10 Determination of the characteristics of the method: sampling and analyse26 10.1 General 26 10.2 Relevant performance characteristics of the method and performance criteria .26 10.2.1 General 26 Licensed Copy: Wang Bin, na, Tue Apr 18 03:14:21 BST

23、2006, Uncontrolled Copy, (c) BSIEN 14791:2005 (E) 4 10.2.2 Sampling procedure .26 10.2.3 Analyse procedure27 10.3 Establishment of the uncertainty budget28 11 Expression of results29 12 Evaluation of the method in the field.31 13 Equivalence of Thorin and ion chromatography methods 31 13.1 General 3

24、1 13.2 Range.31 13.3 Matrix effect.31 13.4 Comparison of repeatability and trueness31 14 Equivalence with an alternative method .31 15 Test report .32 Annex A (informative) Type of sampling equipment33 Annex B (informative) Examples of absorbers.34 Annex C (informative) Example of assessment of comp

25、liance or reference method for SO2with requirements on emission measurements35 Annex D (informative) Evaluation of the method .43 Annex E (informative) Test of equivalency of Thorin method and ion chromatography 50 Annex ZA (informative) Relationship with EU Directives 60 Bibliography.61 Licensed Co

26、py: Wang Bin, na, Tue Apr 18 03:14:21 BST 2006, Uncontrolled Copy, (c) BSIEN 14791:2005 (E) 5 Foreword This European Standard (EN 14791:2005) has been prepared by Technical Committee CEN/TC 264 “Air quality”, the secretariat of which is held by DIN. This European Standard shall be given the status o

27、f a national standard, either by publication of an identical text or by endorsement, at the latest by May 2006, and conflicting national standards shall be withdrawn at the latest by May 2006. This European Standard has been prepared under a mandate given to CEN by the European Commission and the Eu

28、ropean Free Trade Association, and supports essential requirements of EU Directive(s). For relationship with EU Directive(s), see informative Annex ZA, which is an integral part of this European Standard. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the

29、following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, S

30、weden, Switzerland and United Kingdom. Licensed Copy: Wang Bin, na, Tue Apr 18 03:14:21 BST 2006, Uncontrolled Copy, (c) BSIEN 14791:2005 (E) 6 1 Scope This European Standard describes a manual method for sampling and determining SO2content in ducts and stacks emitting to the atmosphere by two analy

31、tical methods: Ion chromatography and Thorin method. This European Standard is the Standard Reference Method (SRM) for periodic monitoring and for calibration or control of Automatic Measuring Systems (AMS) permanently installed on a stack, for regulatory purposes or other purposes. To be used as th

32、e SRM, the user shall demonstrate that the performance characteristics of the method are better than the performance criteria defined in this European Standard and that the overall uncertainty of the method is less than 20,0 % relative at the daily Emission Limit Value (ELV). An Alternative Method t

33、o this SRM may be used provided that the user can demonstrate equivalence according to the Technical Specification CEN TS 14793, to the satisfaction of his national accreditation body or law. This Standard Reference Method has been evaluated during field tests on waste incineration, co-incineration

34、and large combustion installations. It has been validated for sampling periods of 30 min in the range of (0,5 to 2 000) mg/m3SO2for Ion Chromatography variant and 5 mg/m3to 2 000 mg/m3SO2for Thorin method according to emission limit values laid down in the following Council Directives: Council Direc

35、tive 2001/80/EC on the limitation of emissions of certain pollutants into the air from large combustion plants; Council Directive 2000/76/EC on waste incineration plants. The limit values of EU Directives are expressed in mgSO2/m3, on dry basis and at the reference conditions of 273 K and 101,3 kPa.

36、 2 Normative references The following referenced documents are indispensable for the application of this European Standard. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ENV 13005, Guide

37、 to the expression of uncertainly in measurement. EN 13284-1, Stationary source emissions Determination of low range mass concentration of dust Part 1: Manual gravimetric method. CEN/TS 14793, Stationary source emission Intralaboratory validation procedure for an alternative method compared to a ref

38、erence method. 3 Terms, definitions, symbols and abbreviations 3.1 Terms and definitions For the purposes of this European Standard, the following terms and definitions apply. 3.1.1 absorber device in which sulphur oxide is absorbed into an absorption liquid Licensed Copy: Wang Bin, na, Tue Apr 18 0

39、3:14:21 BST 2006, Uncontrolled Copy, (c) BSIEN 14791:2005 (E) 7 3.1.2 absorption efficiency () ratio of quantity of the analyte q1collected in the first absorber divided by the quantity of the analyte collected in the first and the second absorber (q1 + q2) = q1/ (q1+ q2) 3.1.3 analytical detection

40、limit (LD) concentration value of the measurand below which there is at least 95 % level of confidence that the measured value corresponds to a sample free of that measurand 3.1.4 automatic measuring system (AMS) measuring system permanently installed on site for continuous monitoring of emissions N

41、OTE 1 An AM is a method which is traceable to a reference method. NOTE 2 Apart from the analyser, an AMS includes facilities for taking samples (e.g. probe, sample gas lines, flow meters, regulators, delivery pumps) and for sample conditioning (e.g.dust filter, moisture removal devices, converters,

42、diluters). This definition also includes testing and adjusting devices, that are required for regular functional checks. 3.1.5 calibration of an AMS statistical relationship between values of the measurand indicated by the measuring system (AMS) and the corresponding values given by the standard ref

43、erence method (SRM) used during the same period of time and giving a representative measurement on the same sampling plane NOTE The result of calibration permits to establish the relationship between the values of the SRM and the AMS (calibration function). 3.1.6 calibration of the SRM set of operat

44、ions that establish, under specified conditions, the relationship between values of quantities indicated by a measuring instrument or measuring system, and the corresponding values realized by standard reference methods implemented in the state of the art in order to provide representative results V

45、IM 3.1.7 chemical blank value sulphate ion content of an unexposed sample of the absorption solution, plus reagents that are added to the solution before analysis if necessary 3.1.8 emission limit value (ELV) emission limit value according to EU Directives on the basis of 30 min, 1 h or 1 day 3.1.9

46、field blank value determined by a specific procedure used to ensure that no significant contamination has occurred during all steps of the measurement and to check that the operator can achieve a quantification level adapted to the task Licensed Copy: Wang Bin, na, Tue Apr 18 03:14:21 BST 2006, Unco

47、ntrolled Copy, (c) BSIEN 14791:2005 (E) 8 3.1.10 influence quantity quantity that is not the measurand but that affects the result of the measurement adapted VIM 2.7 Examples ambient temperature; atmospheric pressure; presence of interfering gases in the flue gas matrix. 3.1.11 measurand particular

48、quantity subject to measurement VIM 2.6 3.1.12 measurement series several successive measurements carried out on the same sampling plane and at the same process operating conditions EN 13284-1 3.1.13 measuring system complete set of measuring instruments and other equipment assembled to carry out sp

49、ecified measurements VIM 4.5 3.1.14 performance characteristic one of the quantities (described by values, tolerances, range, ) assigned to equipment in order to define its performance Licensed Copy: Wang Bin, na, Tue Apr 18 03:14:21 BST 2006, Uncontrolled Copy, (c) BSIEN 14791:2005 (E) 9 3.1.15 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 Repeatability conditions include: same measur