1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS ISO 11709:2011Soil quality Determinationof selected coal-tar-derivedphenolic compounds usinghigh performance liquidchromatography (HPLC)BS ISO 11709:2011 BRITISH STANDARDNatio
2、nal forewordThis British Standard is the UK implementation of ISO 11709:2011.The UK participation in its preparation was entrusted to TechnicalCommittee EH/4, Soil quality.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purpo
3、rt to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2011ISBN 978 0 580 66862 3ICS 13.080.10Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandard
4、s Policy and Strategy Committee on 31 May 2011.Amendments issued since publicationDate Text affectedBS ISO 11709:2011Reference numberISO 11709:2011(E)ISO 2011INTERNATIONAL STANDARD ISO11709First edition2011-05-15Soil quality Determination of selected coal-tar-derived phenolic compounds using high pe
5、rformance liquid chromatography (HPLC) Qualit du sol Dosage dune slection de composs phnoliques drivs du goudron de houille en utilisant la chromatographie liquide haute performance (CLHP) BS ISO 11709:2011ISO 11709:2011(E) COPYRIGHT PROTECTED DOCUMENT ISO 2011 All rights reserved. Unless otherwise
6、specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISOs member body in the country of the requester. ISO copyright offi
7、ce 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 2011 All rights reservedBS ISO 11709:2011ISO 11709:2011(E) ISO 2011 All rights reserved iiiContents Page Foreword iv 1 Scope1 2 Normative referenc
8、es1 3 Terms and definitions .2 4 Principle .3 5 Interferences 3 5.1 Interference with sampling and extraction .3 5.2 Interferences with the HPLC 3 6 Reagents 3 6.1 General .3 6.2 Mobile phase for HPLC .3 6.3 Extraction .3 6.4 Standards .4 6.5 Preparation of standard solutions.4 7 Apparatus.5 7.1 Ext
9、raction procedures 5 7.2 High performance liquid chromatograph (HPLC) 5 8 Sampling and preservation of samples 6 9 Procedure.6 9.1 Blank test .6 9.2 Extraction .6 9.3 Liquid chromatography 6 9.3.1 General .6 9.3.2 Chromatographic separation .7 9.3.3 Detection 7 9.3.4 Identification of individual com
10、pounds 7 9.3.5 Calibration7 10 Calculation and expression of results 8 11 Test report9 Annex A (informative) Example of chromatographic conditions and chromatogram.10 Annex B (informative) Emission spectrum (FLD, 280 nm to 900 nm) recorded with FLD Agilent 1100.14 Annex C (informative) Ultraviolet s
11、pectrum (DAD, 200 nm to 350 nm), recorded with Dionex UVD 320S 16 Annex D (informative) Examples of limits of determinations of coal-tar-derived phenols for different HPLC detectors 19 Bibliography20 BS ISO 11709:2011ISO 11709:2011(E) iv ISO 2011 All rights reservedForeword ISO (the International Or
12、ganization for Standardization) is a worldwide federation 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 establ
13、ished has the right to be represented on that committee. 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 standardizati
14、on. International Standards are drafted in accordance 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.
15、 Publication as an International Standard requires approval 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 pa
16、tent rights. ISO 11709 was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical methods and soil characteristics. BS ISO 11709:2011INTERNATIONAL STANDARD ISO 11709:2011(E) ISO 2011 All rights reserved 1Soil quality Determination of selected coal-tar-derived phenolic
17、compounds using high performance liquid chromatography (HPLC) 1 Scope This International Standard specifies a method for the quantitative determination of selected coal-tar-derived phenols, namely phenol, methylphenols such as (ortho-, meta-, para-)cresols, and dihydroxybenzenes such as catechol, re
18、sorcinol and hydroquinone (see Table 1) in soil by using high performance liquid chromatography with ultraviolet/diode array (HPLC/UV/DAD) or fluorescence (HPLC/FLD) or electrochemical detection (HPLC/ELCD). It is applicable to all types of soil with contamination levels of individual phenols in the
19、 range of approximately 0,08 mg/kg to 10 mg/kg of soil. NOTE Also with this method, other higher methylated phenols, for example, dimethylphenols such as (2,3-, 2,4-, 2,5-, 2,6-, 3,4- and 3,5-)xylenoles, 2-isopropylphenol, 2,3,5-trimethylphenol and 1-naphthol can be analysed, provided the suitabilit
20、y and the validity of the method are proven. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any am
21、endments) applies. ISO 10381-1, Soil quality Sampling Part 1: Guidance on the design of sampling programmes ISO 11465, Soil quality Determination of dry matter and water content on a mass basis Gravimetric method ISO 8466-1, Water quality Calibration and evaluation of analytical methods and estimati
22、on of performance characteristics Part 1: Statistical evaluation of the linear calibration function BS ISO 11709:2011ISO 11709:2011(E) 2 ISO 2011 All rights reserved3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 coal-tar-derived phenols mono
23、hydroxybenzene, monomethylphenols and dihydroxybenzenes NOTE See Table 1 for details. Table 1 Target phenolic compounds Compounds Molecular formula Molecular mass g/mol CAS-RNaChemical structure Phenol monohydroxybenzene C6H6O 94,11 108-95-2 o-Cresol 2-methylphenol C7H8O 108,14 95-48-7 m-Cresol 3-me
24、thylphenol C7H8O 108,14 108-39-4 p-Cresol 4-methylphenol C7H8O 108,14 106-44-5 o-Dihydroxybenzene 1,2-Dihydroxybenzene (catechol) C6H6O2110,10 120-80-9 m-Dihydroxybenzene 1,3-Dihydroxybenzene (resorcinol) C6H6O2110,10 123-31-9 p-Dihydroxybenzene 1,4-Dihydroxybenzene (hydroquinone) C6H6O2110,10 108-4
25、6-3 aCAS-RN Chemical Abstracts Services-Registry Number. BS ISO 11709:2011ISO 11709:2011(E) ISO 2011 All rights reserved 34 Principle A sample of “as-received” or field-moist soil is extracted with methanol at low pH. Reversed-phase high performance liquid chromatography (HPLC) with direct injection
26、 of a definite extract volume and an appropriate detection technique, such as UV/DAD or fluorescence or electrochemical detection, is used to determine the phenolic compound content. 5 Interferences 5.1 Interference with sampling and extraction Standard laboratory glassware, appropriately cleaned an
27、d free of interfering compounds. Do not use any kind of plastics containers, since the phenols may be adsorbed onto these. Plastics materials may also contribute their impurities to the sample material. 5.2 Interferences with the HPLC Substances which have the same or nearly the same retention time
28、of the target analytes, and which give UV, fluorescence or electrochemical (amperometric) signals, may interfere with the determination. 6 Reagents 6.1 General During the analysis, unless otherwise stated, use only reagents of recognized analytical grade. Solvents for HPLC shall be of the purity rec
29、ommended by the HPLC manufacturer. Only commercially available certified standards of high purity shall be used. WARNING Phenols are both toxic and corrosive and should be handled with care. Methanol and acetonitrile are toxic and acetic acid is corrosive. Latex or nitrile gloves and eye protection
30、should be worn at all times. Spills should immediately be wiped up with adsorbent tissue and placed in sealed containers used for the disposal of toxic chemicals. Samples should be treated as toxic and harmful. 6.2 Mobile phase for HPLC 6.2.1 Water, ultra-pure water is required (HPLC-purity grade).
31、6.2.2 Acetonitrile, C2H3N, HPLC-purity grade. 6.2.3 Acetic acid, CH3COOH, analytical grade. 6.2.4 Helium, He, of suitable purity for degasification of solvents. 6.3 Extraction 6.3.1 Methanol, CH3OH, analytical grade. 6.3.2 Acetic acid, CH3COOH, analytical grade. BS ISO 11709:2011ISO 11709:2011(E) 4
32、ISO 2011 All rights reserved6.3.3 Acidic methanol, 0,1 % volume fraction of acetic acid (6.3.2) in methanol (6.3.1), for the preparation of standard solutions and the extraction. 6.4 Standards 6.4.1 Reference substances (Table 1) Certified solutions of phenols and single-solid phenol substances with
33、 certified purity are available from a limited number of suppliers. 6.4.2 Quality-control standard For example, 4-fluorophenol (CAS 371-41-5). This quality-control standard shall be used to verify the stability of the detection system, especially for ELCD measurements and also for the recovery check
34、 of the extraction. A recovery control check shall be made by addition of a suitable phenolic compound (not mentioned in the scope) to the sample before extraction, which is not interfering with the target analytes, e.g. 4-fluorophenol. 6.5 Preparation of standard solutions 6.5.1 Preparation of cali
35、bration solution of phenols 6.5.1.1 Single-substance stock solutions Prepare solutions of the single substances (see Table 1) and also the quality-control standard in acidic methanol (6.3.3) with a mass concentration of, for example, 10 mg/ml. These solutions are used for confirmation and identifica
36、tion of single phenols in the chromatogram. Weigh, for example, 10 mg of single-solid phenol substances into a 10 ml volumetric flask and fill up to the mark with acidic methanol (6.3.3). 6.5.1.2 Multiple-substance stock solution Prepare the multiple-substance stock solution by mixing appropriate vo
37、lumes of single-substance stock solutions (6.5.1.1) in acidic methanol (6.3.3). The solutions 6.5.1.1 to 6.5.1.2 are stable for at least 6 weeks when stored in the dark at 4 C to 7 C and protected from evaporation. 6.5.1.3 Calibration solutions Prepare at least five calibration solutions by appropri
38、ate dilution of the multiple-substance stock solution (6.5.1.2), using acidic methanol (6.3.3). Transfer, for example, 100 l of the stock solution and a constant volume of quality-control standard solution (6.5.2) into a graduated 10 ml flask and fill up to the mark. 1 l of the calibration solutions
39、 contain 0,5 ng to 5 ng of the respective individual substances. Check the stability of the calibration solutions regularly. NOTE Checking the mass concentration of the phenols in the stock solution is only possible by comparison with an independent, preferably certified, standard solution. BS ISO 1
40、1709:2011ISO 11709:2011(E) ISO 2011 All rights reserved 56.5.2 Preparation of quality-control standard solution Weigh 25 mg of 4-fluorophenol in 50 ml of acidic methanol (6.3.3) in a volumetric flask. The same volume of quality-control standard solution shall be used for calibration and for the samp
41、les. 6.5.3 Preparation of mobile phase Transfer, for example, 1 ml of acetic acid (6.2.3) into a 1 l volumetric flask and fill up to the mark with water (6.2.1). 7 Apparatus Usual laboratory apparatus and in particular the following. 7.1 Extraction procedures Customary laboratory glassware. All glas
42、sware and material that comes into contact with the sample or extract shall be thoroughly cleaned. 7.1.1 Glass sample bottles, equipped with a glass stopper or screw cap and a polytetrafluorethene (PTFE) seal. Size in agreement with the amount of sample taken, e.g. 20 ml vials with a screw cap. 7.1.
43、2 Shaking device, shaking machine with horizontal movement (200 to 300 strokes/min). 7.1.3 Pipettes, of 1 ml and 10 ml (ISO 648, class A), and Pasteur pipettes. 7.1.4 Volumetric flasks, of different volumes, e.g. 10 ml, 100 ml or 1 000 ml (ISO 1042, class A). 7.1.5 Syringes, 50 l, 100 l and 500 l. 7
44、.1.6 Luer lock syringe with micro-membrane filter, e.g. PTFE-membrane, pore size 0,2 m to 0,45 m, for filtration of the HPLC extracts. 7.2 High performance liquid chromatograph (HPLC) 7.2.1 HPLC system An HPLC system equipped according to requirements with either an ultraviolet or a fluorimetric or
45、an electrochemical detection system and a data evaluation system, including a degassing assembly, e.g. for degassing with vacuum or helium, analytical pumps, isocratic or gradient elution, a sample injection system, a column thermostat, capable of keeping the temperature constant to within 0,5 C, a
46、fluorescence detector, including damping/amplification, preferably equipped with monochromator(s), or a UV detector (with variable wavelength) or diode array, or an electrochemical detector for the DC amperometry mode with, for example, an appropriate electrode system. BS ISO 11709:2011ISO 11709:201
47、1(E) 6 ISO 2011 All rights reserved7.2.2 Analytical separation column Use a reversed-phase HPLC column meeting the separation requirements given in the experimental conditions (see Annex D for example). The analytical column can be protected using a guard column. When using guard columns, it is reco
48、mmended to use column connectors with a low dead volume. 8 Sampling and preservation of samples Take samples in accordance with ISO 10381-1. Place the samples as received in glass bottles with PTFE caps. It is recommended to fill the bottles completely. As phenols in soil are subject to biodegradati
49、on, the sample containers should be filled on site to preserve the phenols. Bottles containing reagent should be pre-weighed in the laboratory before being filled with sample material and re-weighed on receipt in the laboratory. Store the samples in the dark in the laboratory at either 18 C or 4 C. Phenols can be subject to microbial conversion under certain conditions. It is recommended that samples be frozen if they are stored for more than 2 days. Samples can be stored for one week at a
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