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1、 Reference number ISO 11338-2:2003(E) ISO 2003 INTERNATIONAL STANDARD ISO 11338-2 First edition 2003-06-01 Stationary source emissions Determination of gas and particle-phase polycyclic aromatic hydrocarbons Part 2: Sample preparation, clean-up and determination missions de sources fixes Dterminatio
2、n des hydrocarbures aromatiques polycycliques sous forme gazeuse et particulaire Partie 2: Prparation des chantillons, purification et dtermination Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/16/2007
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6、roblem relating to it is found, please inform the Central Secretariat at the address given below. ISO 2003 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and micr
7、ofilm, without permission in writing from either ISO at the address below or ISOs member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2
8、003 All rights reserved Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/16/2007 10:05:19 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 11338-2:2003(E) ISO 2003 All rights
9、reserved iii Contents Page Forewordiv Introduction v 1 Scope1 2 Normative references .1 3 Terms and definitions.1 4 Principle.2 4.1 Sampling2 4.2 Analysis2 5 Safety measures2 6 Procedures 2 6.1 HPLC method 2 6.2 GC-MS method 9 7 Limitations and interferences16 7.1 Limitations.16 7.2 Interferences17
10、Annex A (informative) Maximum UV absorption wavelength and recommended combinations of excitation-emission wavelengths for HPLC.18 Annex B (informative) Formulae and physical properties of selected PAH.19 Annex C (informative) Characteristic ions for GC-MS detection of selected PAH, recovery, and su
11、rrogate recovery standards20 Annex D (informative) Applicability of internal standards for GC-MS detection of selected PAH.21 Annex E (normative) Summary of performance characteristics of the HPLC method .22 Bibliography .23 Copyright International Organization for Standardization Provided by IHS un
12、der license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/16/2007 10:05:19 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 11338-2:2003(E) iv ISO 2003 All rights reserved Foreword ISO (the International Organization for Standardization) is a worldwide federa
13、tion of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committ
14、ee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance
15、 with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires ap
16、proval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 11338-2 was prepared by Technical Co
17、mmittee ISO/TC 146, Air quality, Subcommittee SC 1, Stationary source emissions. ISO 11338 consists of the following parts, under the general title Stationary source emissions Determination of gas and particle-phase polycyclic aromatic hydrocarbons: Part 1: Sampling Part 2: Sample preparation, clean
18、-up and determination Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/16/2007 10:05:19 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 11338-2:2003(E) ISO 2003 All rights re
19、served v Introduction This part of ISO 11338 describes procedures for sample preparation, clean-up and analysis of polycyclic aromatic hydrocarbons (PAHs) (collected from stack and waste gases), based on either high performance liquid chromatography (HPLC) (see Annexes A and E) or gas chromatography
20、-mass spectrometry (GC-MS) (see Annexes B, C and D). PAHs are emitted to the atmosphere primarily by the combustion of fossil fuels and wood. PAHs are considered to be an important class of environmental carcinogens. The identification and quantification of PAHs emitted from stationary sources repre
21、sent a critical aspect in the assessment of air quality. Stack and waste gases emitted from stationary sources often contain solid particles. Because of the range of their vapour pressures, PAHs are distributed between gas and particle phases. In the atmosphere, PAHs containing four or more rings te
22、nd to adsorb onto particles, while PAHs containing two to four rings tend to be present in gaseous form. However in stack and waste gases, the distribution of PAHs between gas and particle phases depends on the temperature, the mass of emitted particles, particle size, humidity, type and concentrati
23、on of PAH. During sampling, sample storage and preparation of the sample, losses of PAH can occur and prevent quantitative analysis. These losses can be the result of the volatility of two- and three-ring PAHs, the physical- chemical instability of PAHs in the presence of light, O3, NOx, SO2, HCl an
24、d certain heavy metals. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/16/2007 10:05:19 MDTNo reproduction or networking permitted without license from IHS -,-,- Copyright International Organization for
25、 Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/16/2007 10:05:19 MDTNo reproduction or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARD ISO 11338-2:2003(E) ISO 2003 All rights reserved 1 Stationary source emissions De
26、termination of gas and particle-phase polycyclic aromatic hydrocarbons Part 2: Sample preparation, clean-up and determination 1 Scope This part of ISO 11338 specifies procedures for sample preparation, clean-up and analysis for the determination of gas and particle-phase polycyclic aromatic hydrocar
27、bons (PAH) in stack and waste gases. The analytical methods are capable of detecting sub-microgram concentrations of PAH per cubic metre of sample, depending on the type of PAH and the flue gas volume sampled. The methods described in this part of ISO 11338 are based on either high performance liqui
28、d chromatography (HPLC) or gas chromatography-mass spectrometry (GC-MS). NOTE ISO 11338-1 describes three methods and specifies minimum requirements for the sampling of PAH in stack and waste gases. 2 Normative references The following referenced documents are indispensable for the application of th
29、is document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 4225:1994, Air quality General aspects Vocabulary 3 Terms and definitions For the purposes of this document, the terms and
30、definitions given in ISO 4225 and the following apply. 3.1 polycyclic aromatic hydrocarbon PAH compound that contains two or more fused aromatic rings made up of carbon and hydrogen atoms 3.2 stationary source emission gas emitted by a stationary plant or process and transported to a chimney for dis
31、persion into the atmosphere 3.3 accelerated solvent extractor ASE equipment that accelerates the traditional extraction process by using solvent at elevated temperatures NOTE Pressure is applied to the sample extraction cell to maintain the heated solvent in a liquid state during the extraction. Cop
32、yright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/16/2007 10:05:19 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 11338-2:2003(E) 2 ISO 2003 All rights reserved 4 Principle 4.1
33、Sampling A representative sample is collected from the gas passing through a duct under isokinetic conditions with the use of a suitable sampling device. The particulate phase is collected on a suitable filter and the gas phase is trapped by condensation onto an adsorbent e.g. styrene-divinylbenzene
34、 polymer resin (XAD-2), polyurethane foam or other adsorbent of comparable efficiency. 4.2 Analysis After sampling, the sample is removed from the sampling equipment. The parts of the sampling equipment which have been in contact with the sample are washed with solvent. The washings are then combine
35、d with the filter(s) and adsorbent and then extracted with a suitable organic solvent, with the use of a Soxhlet extractor or other validated method, e.g. accelerated solvent extractor (ASE). The extract is concentrated by means of a rotary evaporator, followed by further concentration under nitroge
36、n if necessary. Sample clean-up may be necessary before quantification. An aliquot of the concentrated sample is analysed either by reversed phase high performance liquid chromatography (HPLC) or by gas chromatography-mass-spectrometry (GC-MS). The concentration of each PAH is calculated from the ma
37、ss of PAH (particle- and gas-phase) determined during analysis and the volume of flue gas sampled corrected to appropriate reference conditions. 5 Safety measures All PAH should be treated as potential carcinogens. The user should be familiar with the chemical and physical properties of PAH. Measure
38、s shall be taken to prevent PAH in solid form, extract or solution coming into contact with the body. PAH can co-distil with the solvent and may cling to the outside of glassware with ground glass stoppers. Owing in particular to the risks associated with working with PAH in solid form, self-prepara
39、tion of standard solutions is ill-advised. The use of commercially available standard solutions1) minimizes the risk of exposure. All glassware containing PAH solutions shall therefore be handled with solvent-resistant gloves. Any contamination can be revealed in ultraviolet light by fluorescence. P
40、AH are most dangerous in solid form, becoming electrostatically charged. Therefore PAH should be weighed in a glove box. Unused samples and contaminated equipment, glassware and clothing shall be disposed of properly, taking into account the relevant regulations. 6 Procedures 6.1 HPLC method 6.1.1 G
41、eneral This subclause describes the preparation, sample clean-up and analytical method for determining the concentration of polycyclic aromatic hydrocarbons (PAH) in stack and waste gases using high pressure liquid chromatography (HPLC). 1) Standard Reference Material (SRM) 1647: Priority Pollutant
42、Polynuclear Aromatic Hydrocarbons, a certified solution of 16 PAH in acetonitrile. This solution is an example of a suitable product available commercially from The National Institute of Standards and Technology (NIST), US Department of Commerce, Gaithersburg, MD, USA. This information is given for
43、the convenience of users of this part of ISO 11338 and does not constitute an endorsement by ISO of this product. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/16/2007 10:05:19 MDTNo reproduction or ne
44、tworking permitted without license from IHS -,-,- ISO 11338-2:2003(E) ISO 2003 All rights reserved 3 6.1.2 Reagents and materials 6.1.2.1 Acetonitrile, HPLC grade. 6.1.2.2 n-Hexane, HPLC grade. 6.1.2.3 Methanol, HPLC grade. 6.1.2.4 Pentane, HPLC grade. 6.1.2.5 Diethyl ether, reagent grade, preserved
45、 with 2 % ethanol, HPLC grade. 6.1.2.6 Silica gel, high purity grade, type 60, 70 mesh to 23 mesh. 6.1.2.7 Sodium sulfate, anhydrous, reagent grade, dried by heating at 300 C for at least 4 h. 6.1.2.8 Recovery standards for HPLC: 2-methylchrysene or 6-methylchrysene, purity at least 98 %. 6.1.2.9 Co
46、mpressed gases: high purity helium for degassing the mobile phase and high purity nitrogen for sample concentration. 6.1.2.10 Aluminium foil. 6.1.2.11 Glass wool. 6.1.3 Apparatus 6.1.3.1 Soxhlet extractor, capacity 100 ml to 200 ml, and appropriate condenser. 6.1.3.2 Glass-fibre filter, precleaned b
47、y heating for 3 h at 200 C or to an acceptable blank level. 6.1.3.3 Round-bottom flasks, capacity 100 ml and either 250 ml or 500 ml depending on the capacity of the Soxhlet extractor. 6.1.3.4 Rotary evaporator system, capable of producing a maximum vacuum of 0,1 MPa (1,0 bar), and with a water bath
48、 that can be heated to 50 C. 6.1.3.5 Kuderna Danish concentrators, capacity 500 ml, including 10 ml graduated concentrator tubes with ground-glass stoppers, and a 3-ball macro-Snyder column. 6.1.3.6 Nitrogen evaporative concentrator: nitrogen blow-down apparatus with flowrate control and temperature-controlled water bath, evaporator tubes of volume 1 ml to 10 ml. 6.1.3.7 Separation funnels, of capacity 100 ml and 250 ml. 6.1.3.8 Glass chromatography column. 6.1.3.9 C