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1、BRITISH STANDARD BS EN 13649:2002 Stationary source emissions Determination of the mass concentration of individual gaseous organic compounds Activated carbon and solvent desorption method The European Standard EN 13649:2001 has the status of a British Standard ICS 13.040.40 NO COPYING WITHOUT BSI P
2、ERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Licensed Copy: sheffieldun sheffieldun, na, Sun Oct 29 09:05:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN 13649:2002 This British Standard, having been prepared under the direction of the Health and Environment Sector Policy and Strategy Committe
3、e, was published under the authority of the Standards Policy and Strategy Committee on 4 February 2002 BSI 4 February 2002 ISBN 0 580 39001 2 National foreword This British Standard is the official English language version of EN 13649:2001. The UK participation in its preparation was entrusted by Te
4、chnical Committee EH/2, Air quality, to Subcommittee EH/2/1, Stationary source emissions, which has the responsibility to: A list of organizations represented on this subcommittee can be obtained on request to its secretary. Cross-references The British Standards which implement international or Eur
5、opean publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the nec
6、essary provisions of a contract. Users of British Standards are responsible for their 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 European committee any enquiries o
7、n the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the EN title page, pages 2 to 21 and a back cover.
8、The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments Licensed Copy: sheffieldun sheffieldun, na, Sun Oct 29 09:05:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPI
9、SCHE NORM EN 13649 November 2001 ICS 13.040.40 English version Stationary source emissions - Determination of the mass concentration of individual gaseous organic compounds - Activated carbon and solvent desorption method Emissions de sources fixes - Dtermination de la concentration massique en comp
10、oss organiques gazeux individuels - Mthode par charbon actif et dsorption des solvants Emissionen aus stationren Quellen - Bestimmung der Massenkonzentration von einzelnen gasfrmigen organischen Verbindungen - Aktivkohleadsorptions- und Lsemitteldesorptionsverfahren This European Standard was approv
11、ed by CEN on 29 September 2001. 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. Up-to-date lists and bibliographical references concerning such nationa
12、l standards may be obtained on application to the Management Centre or to any CEN member. This European Standard exists 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 notifie
13、d to the Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and Un
14、ited Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2001 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 13649:200
15、1 E Licensed Copy: sheffieldun sheffieldun, na, Sun Oct 29 09:05:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13649:2001 (E) 2 Contents page Foreword3 1Scope3 2Normative references3 3Terms and definitions4 4Principle4 5Apparatus and materials5 6Sampling procedure9 7Analytical procedure11 8Calcul
16、ation13 9Report13 Annex A (informative) Measurement uncertainty and associated statistics15 Annex B (informative) Typical desorption efficiencies of selected organic components on activated carbon17 Annex C (informative) Procedure for control of leakage19 Annex D (informative) Procedure for dilution
17、 sampling20 Annex E (informative) Safety measures21 Licensed Copy: sheffieldun sheffieldun, na, Sun Oct 29 09:05:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13649:2001 (E) 3 Foreword This European Standard has been prepared by Technical Committee CEN/TC 264 “Air Quality“, the secretariat of whi
18、ch is held by DIN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by May 2002, and conflicting national standards shall be withdrawn at the latest by May 2002. This European Standard has been prepar
19、ed under a mandate given to CEN by the European Commission and European Free Trade Association. The annexes A, B, C, D and E are informative. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standa
20、rd: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. 1Scope This European Standard specifies procedures for the sampling onto activated carbon, the prepa
21、ration and the analysis of samples of volatile organic components such as those arising from solvent using processes. It can be used as a reference method. NOTE See Council Directive 1999/13/EEC. The results obtained using this Standard are expressed as the mass concentration (mg/m3) of the individu
22、al gaseous organic components. This Standard is suitable for use in the range of about 0,5 mg/m3 to 2000 mg/m3. For the measurement of the mass concentration of total organic carbon arising from solvent using processes then EN 13526 should be used. 2Normative references This European Standard incorp
23、orates, by dated or undated reference, provisions from other publications. These normative references are cited at the appropriate places in the text, and the publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this Eur
24、opean Standard only when incorporated in it by amendment or revision. For undated references the latest edition of the publication referred to applies (including amendments). Licensed Copy: sheffieldun sheffieldun, na, Sun Oct 29 09:05:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13649:2001 (E)
25、4 EN 13526:2001, Stationary source emissions - Determination of the mass concentration of total gaseous organic carbon in flue gases from solvent using processes - Continuous flame ionisation detector method. ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results Part 1: Ge
26、neral principles and definitions. ISO 9169, Air Quality Determination of performance characteristics of measurement methods. 3Terms and definitions For the purposes of this European Standard the following terms and definitions apply. 3.1 desorption efficiency ratio of the mass of the recovered organ
27、ic material to the mass of organic material added to the carbon adsorbent expressed as a percentage 3.2 detection limit minimum concentration of a substance which produces an observable response, as referred to in ISO 9169 3.3 dilution gas gas used to dilute sampled flue gas to prevent water condens
28、ation 3.4 flue gas gaseous waste product from a solvent using process 4Principle 4.1 General There are three steps in the measurement of individual gaseous organic components. They are flue gas sampling, the treatment of sampled material, and the chemical analysis by gas chromatography. 4.2 Flue gas
29、 sampling The principles of sampling are as follows: - Organic components from a measured volume of gas shall be adsorbable onto the activated carbon. - Particulate material which might interfere with the measurement should be removed. Licensed Copy: sheffieldun sheffieldun, na, Sun Oct 29 09:05:35
30、GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13649:2001 (E) 5 - Water condensation should be prevented. 4.3 Treatment of sampled material The collected organic material shall be desorbed using an extraction solvent. 4.4 Chemical analysis An aliquot of the sample is injected into a gas chromatograph
31、y system equipped with a capillary column and an appropriate detector (e.g. flame ionisation detector, mass selective detector etc.). The components are separated by gas chromatography. The detector signals are evaluated using the calibration function. 4.5 Desorption efficiency determination At the
32、sample preparation stage a known amount of a reference material is introduced on to a blank carbon tube to determine component desorption efficiency. The desorption efficiency can be determined as shown in annex B. NOTE The desorption efficiency should be better than 80 %. 5Apparatus and materials 5
33、.1 Sampling system general aspects The sampling system shall be designed to take account of the flue gas characteristics: -it shall be made of a material that is chemically and physically inert to the constituents of the flue gas; NOTE 1 Stainless steel, glass, polytetrafluoroethylene and polypropyl
34、enefluoride are well proven construction materials. -the sampling line shall be as short as possible; -the sampling line shall include a filtering device directly after the probe to trap particles; -it shall be designed to prevent condensation. NOTE 2 Many of the solvent using processes covered by t
35、he Council Directive 1999/13/EEC produce flue gases which do not have a high water content. Where high solvent concentrations or the condensation of water vapour is expected this CEN Standard recommends the use of dilution sampling systems. Licensed Copy: sheffieldun sheffieldun, na, Sun Oct 29 09:0
36、5:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13649:2001 (E) 6 Examples of systems suitable for sampling both dry and wet flue gases are described in this standard. 5.1.1 Sampling without dilution An example of a suitable sampling system is shown in Figure 1. ? 123 4 56 7 8 1Prefilter/sampling
37、probe unit 2Sample line 3Sorbent tube 4Drying unit 5Adjustment Valve 6Pump 7Flow meter 8Gas meter Figure 1 - Example of a flue gas sampling system 5.1.2 Sampling using dynamic dilution An example of a dynamic dilution system is shown in Figure 2. The dilution should be adjustable and shall be consta
38、nt to within 5 % during operation. ? 123 4 56 7 8 1Prefilter/sampling probe unit 2Sample line 3Sorbent tube 4Drying unit 5Adjustment Valve 6Pump 7Flow meter 8Gas meter (total volume) 9Carbon 10Gas meter (dilution volume) ? 10 295 7 6 Figure 2 - Example of a dynamic dilution sampling system Licensed
39、Copy: sheffieldun sheffieldun, na, Sun Oct 29 09:05:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13649:2001 (E) 7 5.1.3 Sampling using static dilution Static dilution sampling can be carried out by part filling a sample bag, fabricated from an inert material, with a known volume of dry dilution
40、gas, a known volume of flue gas is then added. A heated sampling probe can be used to ensure that no condensation occurs before the sample enters the bag. Following sampling the bag is emptied through the sorbent tube. NOTE 1 A suitable procedure is the lung principle in which a sample bag is placed
41、 in a rigid, leak proof container, the air is removed from the container using a vacuum pump, the reduced pressure in the container causes the bag to fill with a volume of sample equal to that which has been removed from the container. A pressure control device operating at not greater than 250 Pa s
42、hould be used to prevent the bag bursting. NOTE 2 A suitable bag material include polyvinyl fluoride. NOTE 3 A suitable procedure for collecting diluted gas samples is given in annex D. ? 2 1 5 6 3 4 Key 1 PTFE tube 2 Pump 3 Bag (partially filled with dilution gas) 4 Rigid container 5 PTFE valve 6 P
43、ressure control device Figure 3 - Example of a static dilution sampling system Licensed Copy: sheffieldun sheffieldun, na, Sun Oct 29 09:05:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13649:2001 (E) 8 5.1.4 Sorbent tube The sorbent tube, filled with activated carbon as the adsorbent, shall have
44、 the following characteristics: - a main adsorbent layer containing not less than 100 mg of activated carbon; NOTE 1 A suitable material is activated carbon prepared from coconut shell. -a security adsorbent layer to detect breakthrough; -the sorbent tube construction material shall be inert; NOTE 2
45、 A suitable material is glass. - the sorbent tubes shall be free from contamination. Open or used sorbent tubes shall not be reused. Sorbent tubes shall be used in accordance with the manufacturers instructions to avoid leakage and sample loss. NOTE 3 Typical desorption efficiencies of common solven
46、ts from tubes of this type are given in annex B. 5.1.5 Dilution gas Dilution gas should be nitrogen or dry air containing less than 0.1 % of the emission limit value of any of the principal components under investigation. NOTE Nitrogen of purity 99,999 % or ambient air, purified by passage through a
47、ctivated carbon, normally meets these requirements. 5.2 Analytical reagents 5.2.1 General Only reagents of recognised analytical grade or better quality shall be used. 5.2.2 Extraction Solvent Extraction solvents shall be of chromatographic quality and free from components co-eluting with the compon
48、ents of interest. NOTE 1 Carbon disulphide (CS2) is a suitable extraction solvent for most of the components likely to be encountered in solvent using processes. NOTE 2 For polar substances other extraction solvents can be used (see annex B). Licensed Copy: sheffieldun sheffieldun, na, Sun Oct 29 09
49、:05:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13649:2001 (E) 9 5.2.3 Reference materials for calibration of the analytical procedure The chromatograph shall be calibrated with those reference materials which correspond to the components likely to arise in the process under investigation. For the purpose of calibration the reference materials shall be prepared in a solution of the extraction solvent to be used. The extraction solvents are highly volatile and fresh reference standards should be prepared regularly. 5.3 Analytical apparatu
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