ISO 13859-2014 Soil quality - Determination of polycyclic aromatic hydrocarbons (PAH) by gas chromatography (GC) and high performance liquid chromatography (HPL.pdf
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1、 ISO 2014 Soil quality Determination of polycyclic aromatic hydrocarbons (PAH) by gas chromatography (GC) and high performance liquid chromatography (HPLC) Qualit du sol Dtermination des hydrocarbures aromatiques polycycliques (HAP) par chromatographie en phase gazeuse (CPG) et chromatographie liqui
2、de haute performance (CLHP) INTERNATIONAL STANDARD ISO 13859 First edition 2014-02-01 Reference number ISO 13859:2014(E) ISO 13859:2014(E)ii ISO 2014 All rights reserved COPYRIGHT PROTECTED DOCUMENT ISO 2014 All rights reserved. Unless otherwise specified, no part of this publication may be reproduc
3、ed or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below or ISOs member body in the country of the requester. I
4、SO 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 ISO 13859:2014(E) ISO 2014 All rights reserved iii Contents Page Foreword iv Introduction v 1 Scope . 1 2 Normative references 2 3 T erm
5、s and definitions . 2 4 Principle 3 5 Interferences 3 5.1 Interference with sampling and extraction 3 5.2 Interference with GC-MS 4 5.3 Interferences with the HPLC . 4 6 Safety remarks 4 7 Reagents 5 7.1 General . 5 7.2 Reagents for extraction 5 7.3 Reagents for clean-up 5 7.4 Reagents for chromatog
6、raphic analysis 6 7.5 Standards . 7 7.6 Preparation of standard solutions . 8 7.7 Preparation of internal standard solutions 9 7.8 Preparation of injection standard solution 9 8 Apparatus . 9 9 Sample storage and preservation 11 9.1 Sample storage .11 9.2 Sample pretreatment 11 10 Procedure11 10.1 B
7、lank test 11 10.2 Extraction .12 10.3 Concentration or dilution .14 10.4 Clean-up of the extract 15 10.5 Addition of the injection standard 16 10.6 Gas chromatographic analysis (GC) .17 10.7 High performance liquid chromatographic analysis (HPLC) .20 11 Performance characteristics .23 12 Precision 2
8、3 13 Test report 23 Annex A (informative) Repeatability and reproducibility data .24 Annex B (informative) Examples of instrumental conditions and chromatograms .27 Bibliography .37 ISO 13859:2014(E) Foreword ISO (the International Organization for Standardization) is a worldwide federation of natio
9、nal 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 committee. Internati
10、onal 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. The procedures used to develop this document and those intende
11、d for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.is
12、o.org/directives). 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. Details of any patent rights identified during the development of the document wil
13、l be in the Introduction and/or on the ISO list of patent declarations received (see www.iso.org/patents). Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement. For an explanation on the meaning of ISO specific terms and expres
14、sions related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary information The committee responsible for this document is ISO/TC 190, Soil quality, Subcommittee SC 3, C
15、hemical methods and soil characteristics.iv ISO 2014 All rights reserved ISO 13859:2014(E) Introduction Polycyclic aromatic hydrocarbons (PAH) are ubiquitous because they are released in appreciable quantities every year into the environment through the combustion of organic matters such as coal, fu
16、el oils, petrol, wood, refuse, and plant materials. Since some of these PAH compounds are carcinogenic or mutagenic, their presence in the environment (air, water, soil, sediment, and waste) is regularly monitored and controlled. At present, determination of PAH is carried out in these matrices in m
17、ost of the routine laboratories following the preceding steps for sampling, pretreatment, extraction, clean-up by measurement of specific PAH by means of gas chromatography in combination with mass spectrometric detection (GC-MS) or by high performance liquid chromatography (HPLC) in combination wit
18、h UV-DAD or fluorescence detection (HPLC-UV-DAD/FLD). Both the GC-MS and the HPLC methods are included in this horizontal standard. It is to be underlined that the target contamination level of PAH can lie in the range of about 0,01 mg/kg per individual PAH (agricultural soil and sediment) to about
19、200 mg/kg and higher (e.g. contaminated soil at coking plant sites or waste). The use of internal and injection standards is described in order to have an internal check on execution of the extraction and clean-up procedure. The method is as far as possible in agreement with the method described for
20、 PCBs (see EN 16167). This International Standard is the result of a desk study “Horizontal International Standard for determination of PAH in sludge, soil, and biowaste” in the project “Horizontal” and aims at evaluating the latest developments in assessing PAH in sludge, soil, treated biowaste, an
21、d neighbouring fields. After an evaluation study, in which the ruggedness of the method was studied, a European-wide validation of the draft standard has taken place. The results of the desk studies as well as the evaluation and validation studies have been subject to discussions with all parties co
22、ncerned in CEN. This International Standard is applicable and validated for several types of matrices as indicated in Table 1 (see also Annex A for the results of the validation). Table 1 Matrices for which this International Standard is applicable and validated Matrix Materials used for validation
23、Sludge Municipal sludge Biowaste Fresh compost ISO 2014 All rights reserved v Soil quality Determination of polycyclic aromatic hydrocarbons (PAH) by gas chromatography (GC) and high performance liquid chromatography (HPLC) WARNING Persons using this International Standard should be familiar with us
24、ual laboratory practice. This International Standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions. IM
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