1、Stationary source emissions Determination of the mass concentration of individual gaseous organic compounds Activated carbon and solvent de sorption method The European Standard EN 13649:2001 has the status ofa British Standard ICs 13.040.40 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY C
2、OPYRIGHT LAW BS EN 13649:2002 BS EN 13649:2002 Amd. No. National foreword Date Comments This British Standard, having been prepared under the direction of the Health and Environment Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee
3、 on 4 February 2002 This British Standard is the official English language version of EN 13649:2001. The UKparticipation in its preparation was entrusted by Technical Committee EH/2, Air quality, to Subcommittee EH/2/1, Stationary source emissions, which has the responsibility to: - - aid enquirers
4、to understand the text; present to the responsible European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. - A list of organizations represented on this
5、 subcommittee can be obtained on request to its secretary. Cr oss-r e fer enc e s The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence I
6、ndex”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself
7、 confer immunity from legal obligations. 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. The BSI copyright date displayed in this document indicates when the document was last issued. O BSI 4 February 2002 ISBN O 580 3
8、9001 2 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE 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 - Dt
9、ermination de la concentration massique en composs 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 Lsemitteldesorpt
10、ionsverfa hren This European Standard was approved by CEN on 29 September 2001 CEN members are bound to comply with the CENKENELEC 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 bibl
11、iographical references concerning such national 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
12、a CEN member into its own language and notified 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, Norwa
13、y, Portugal, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION EUROPISCHES KOMITEE FR NORMUNG COMIT EUROPEN DE NORMALISATION Management Centre: rue de Stassart, 36 B-1050 Brussels O 2001 CEN All rights of exploitation in any form and by any means reserved worldwid
14、e for CEN national Members. Ref. No. EN 13649:2001 E EN 13649:2001 (E) Contents Foreword Scope Normative references Terms and definitions Principle Apparatus and materials Sampling procedure Analytical procedure Calculation Report 3 3 4 4 5 9 11 13 13 Annex A (informative) Measurement uncertainty an
15、d associated statistics 15 Annex B (informative) Typical desorption efficiencies of selected organic components on activated carbon 17 Annex C (informative) Procedure for control of leakage 19 Annex D (informative) Procedure for dilution sampling 20 Annex E (informative) Safety measures 21 2 EN 1364
16、9:2001 (E) Foreword This European Standard 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 of a national standard, either by publication of an identical text or by endorsement, at the latest
17、by May 2002, and conflicting national standards shall be withdrawn at the latest by May 2002. This European Standard has been prepared 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 CENKENELE
18、C Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switz
19、erland and the United Kingdom. 1 Scope This European Standard specifies procedures for the sampling onto activated carbon, the preparation 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 Cou
20、ncil Directive 1999/13/EEC. The results obtained using this Standard are expressed as the mass concentration (mg/m3) of the individual 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 o
21、rganic carbon arising from solvent using processes then EN 13526 should be used. 2 Normative references This European Standard incorporates, by dated or undated reference, provisions from other publications. These normative references are cited at the appropriate places in the text, and the publicat
22、ions are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incorporated in it by amendment or revision. For undated references the latest edition of the publication referred to applies (including amend
23、ments). 3 EN 13649:2001 (E) EN 13526:200 1, Stationary source emissions - Determination of the mass concentration of total gaseous organic carbon in jlue gases from solvent using processes - Continuous jlame ionisation detector method. IS0 5725- 1, Accuracy (trueness and precision) of measurement me
24、thods and results Part 1: General principles and definitions. IS0 9 169, Air Quality - Determination of performance characteristics of measurement methods. 3 Terms and definitions For the purposes of this European Standard the following terms and definitions apply. 3.1 desorption efficiency ratio of
25、 the mass of the recovered organic 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 IS0 9169 3.3 dilution gas gas used to dilute sampled f
26、lue gas to prevent water condensation 3.4 flue gas gaseous waste product from a solvent using process 4 Principle 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
27、 gas chromatography. 4.2 Flue gas 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. 4 EN 13649:2001 (E) - Water con
28、densation 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 chromatography system equipped with a capillary column and an appropriate detector (e.g
29、. 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 sample preparation stage a known amount of a reference material is introdu
30、ced 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 %. 5 Apparatus and materials 5.1 Sampling system - general aspects The sampling system shall be designe
31、d 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 construction materials. Stainless steel, glass, polytetrafluoroethylene and polypropylenefluoride are well proven - the sampling lin
32、e 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 the Council Directive 1999/13/EEC produce flue gases which do not ha
33、ve 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. 5 EN 13649:2001 (E) Examples of systems suitable for sampling both dry and wet flue gases are described in this standard. 5.1.
34、1 Sampling without dilution An example of a suitable sampling system is shown in Figure 1 4 7 Prefilter/sampling probe unit Sample line Sorbent tube Drying unit Adjustment Valve Pump Flow meter Gas meter Figure 1 - Example of a flue gas sampling system 5.1.2 Sampling using dynamic dilution An exampl
35、e of a dynamic dilution system is shown in Figure 2. The dilution should be adjustable and shall be constant to within 5 % during operation. 4 7 1 Prefilter/sampling probe unit 2 Sample line 3 Sorbent tube 4 Drying unit 5 Adjustment Valve 7 Flow meter 8 Gas meter (total volume) 9 Carbon 10 Gas meter
36、 (dilution volume) 7 6 Pump Figure 2 - Example of a dynamic dilution sampling system 6 EN 13649:2001 (E) 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 gas, a known
37、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 in a rigid,
38、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 should be used
39、 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. Key 1 PTFE tube 2 Pump 3 Bag (partially filled with dilution gas) 4 Rigid container 5 PTFE valve 6 Pressure control device Figu
40、re 3 - Example of a static dilution sampling system 7 EN 13649:2001 (E) 5.1.4 Sorbent tube The sorbent tube, filled with activated carbon as the adsorbent, shall have the following characteristics: - a main adsorbent layer containing not less than 1 O0 mg of activated carbon; NOTE 1 A suitable mater
41、ial is activated carbon prepared from coconut shell. - a security adsorbent layer to detect breakthrough; - the sorbent tube construction material shall be inert; NOTE 2 A suitable material is glass. - the sorbent tubes shall be free from contamination. Open or used sorbent tubes shall not be reused
42、. Sorbent tubes shall be used in accordance with the manufacturers instructions to avoid leakage and sample loss. NOTE 3 Typical desorption efficiencies of common solvents 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
43、 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 activated carbon, normally meets these requirements. 5.2 Analytical reagents 5.2.1 General Only reagents of recognised analytical gr
44、ade 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 components of interest. NOTE 1 Carbon disulphide (CS2) is a suitable extraction solvent for most of the components likely to be encounter
45、ed in solvent using processes. NOTE 2 For polar substances other extraction solvents can be used (see annex B). 8 EN 13649:2001 (E) 5.2.3 Reference materials for calibration of the analytical procedure The chromatograph shall be calibrated with those reference materials which correspond to the compo
46、nents 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 Analytica
47、l apparatus Laboratory apparatus suitable for capillary column chromatography shall be used. 6 Sampling procedure 6.1 General Aspects The sample shall be representative of both the process emission and the local distribution of the measured constituents in the sampling plane. The following points sh
48、ould be considered when sampling: - the nature of the plant process e.g. steady state or cyclic. If possible the sampling programme should be carried out under steady operating conditions of the plant; - the expected concentration to be measured and any required averaging period, both of which can i
49、nfluence the sampling time. 6.2 Choice of sampling procedure The choice of sampling procedure shall be governed by the characteristics of the gas. Sampling directly onto the sorbent material can be used when the flue gas does not have a high water content and the mass concentration of (organic) material is such that break through is unlikely to occur. The temperature of the flue gas should not exceed 40 “C during adsorption. Provided that no condensation occurs hotter flue gas can be cooled down using a cooling section (inert sampling line). Sampling using dilution or equivalent
