1、BRITISH STANDARD BS ISO 14154:2005 Soil quality Determination of some selected chlorophenols Gas-chromatographic method with electron-capture detection ICS 13.080.10 BS ISO 14154:2005 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 15 Februar
2、y 2005 BSI 15 February 2005 ISBN 0 580 45445 2 National foreword This British Standard reproduces verbatim ISO 14154:2005 and implements it as the UK national standard. The UK participation in its preparation was entrusted by Technical Committee EH/4, Soil committee, to Subcommittee EH/4/3, Chemical
3、 methods and soil characteristics, 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 publications referred to in this document may be found in the
4、 BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible f
5、or its 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 international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK in
6、terests 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 ISO title page, pages ii to iv, pages 1 to 14, an inside back cover and a back cover. The BSI copyright notice d
7、isplayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date Comments Reference number ISO 14154:2005(E) OSI 5002INTERNATIONAL STANDARD ISO 14154 First edition 2005-02-01Soil quality Determination of some selected chlorophenols Gas-chromato
8、graphic method with electron-capture detection Qualit du sol Dosage de certains chlorophnols Mthode de chromatographie en phase gazeuse avec dtection par capture dlectrons BSISO14154:2005IS:45141 O5002(E) DPlcsid Fremia ihTs PDF file may ctnoian emdebt dedyfepcaes. In ccaocnadrw eith Aebods licensil
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15、aii ISO 5002 Allr ithgsr esedevrBSISO14154:2005IS:45141 O5002(E) I SO 5002 All irthgs ersedevr iiiContents Page Foreword iv 1 Scope 1 2 Normative references . 1 3 Terms and definitions. 1 4 Principle . 2 5 Reagents 2 6 Apparatus. 4 7 Sampling 4 8 Procedure 4 9 Calculation. 6 10 Precision 7 11 Qualit
16、y assurance and control 7 12 Test report 7 Annex A (informative) Typical concentrations of standard solutions. 9 Annex B (informative) Example of gas chromatographic conditions . 10 Annex C (informative) Results of interlaboratory test 11 Bibliography . 14 BSISO14154:2005IS:45141 O5002(E) iv I SO 50
17、02 All irthgs ersedevrForeword ISO (the International Organization 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
18、 subject for which a technical committee has been established 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 Commissio
19、n (IEC) on all matters of electrotechnical standardization. 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 co
20、mmittees are circulated to the member bodies for voting. 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 no
21、t be held responsible for identifying any or all such patent rights. ISO 14154 was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical methods and soil characteristics. BSISO14154:2005INTENRATIONAL TSANDADR IS:45141 O5002(E)I SO 5002 All irthgs ersedevr 1Soil qualit
22、y Determination of some selected chlorophenols Gas-chromatographic method with electron-capture detection WARNING Chlorophenols are toxic and some are even carcinogenic. When handling samples containing chlorophenols, avoid skin contact. Use gloves and protective clothing. If large amounts of aeroso
23、ls and dust particles are produced during the sampling, breathing protection may be necessary. 1 Scope This International Standard describes the gas chromatographic determination of 15 chlorophenols (2,3-, 2,4- 2,5-, 2,6-, 3,4- and 3,5-dichlorophenol; 2,3,4-, 2,3,5-, 2,3,6-, 2,4,5-, 2,4,6- and 3,4,5
24、-trichlorophenol, 2,3,4,5- and 2,3,4,6-tetrachlorophenol and pentachlorophenol) in soil samples. This method can also be applied to other solid samples such as sediments and solid wastes. This International Standard describes an acid-base liquid extraction, followed by acetylation and then liquid/li
25、quid extraction. Determination of mass concentration is then carried out by gas chromatography and electron-capture detection. This method is applicable to chlorophenols at the lowest mass concentrations ranging from approximately 0,01 mg/kg to 0,05 mg/kg depending on the component sensitivity and t
26、he quantity of sample used. In some cases complete separation of isomers cannot be achieved, in which case the sum is reported (for instance 2,4- and 2,5-dichlorophenols). 2 Normative references The following referenced documents are indispensable for the application of this document. For dated refe
27、rences, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 3696:1987, Water for analytical laboratory use Specification and test methods ISO 10381-1, Soil quality Sampling Part 1: Guidance on the design of sam
28、pling programmes ISO 11465:1993, Soil quality Determination of dry matter and water content on a mass basis Gravimetric method ISO 14507, Soil quality Pretreatment of samples for determination of organic contaminants 3 Terms and definitions For the purposes of this document, the following terms and
29、definitions apply. 3.1 chlorophenol aromatic hydroxy compound (phenol) carrying one to five chlorine atoms BSISO14154:2005IS:45141 O5002(E) 2 I SO 5002 All irthgs ersedevr4 Principle The method described here is based on two steps. The first step includes a solid/liquid extraction: the chlorophenols
30、 are extracted from soil by a mixture of acetone-hexane at low pH. The second step is a purification step, based on successive extractions in basic and acidic aqueous media and hexane. Finally, the chlorophenols obtained in an aqueous carbonate solution are derivatized with acetic anhydride; the der
31、ivatives formed are extracted from this sample with hexane. The hexane fraction is analysed by gas chromatography with electron capture or mass detection. 5 Reagents During the analysis, unless otherwise stated, use only reagents of recognized analytical grade. Gases for gas chromatography shall be
32、of a purity as recommended by the gas chromatograph manufacturer. Only commercially available certified standards of high purity shall be used. 5.1 Water of at least grade 1 as defined in ISO 3696:1987 5.2 Ethanol, C 2 H 5 OH, 99,5 % (mass fraction) 5.3 Hexane, C 6 H 145.4 Acetone, CH 3 COCH 35.5 Hy
33、drochloric acid, HCl, concentrated, 37 % (mass fraction) 5.6 Sodium hydroxide, NaOH 5.7 Potassium carbonate, K 2 CO 35.8 Acetic anhydride, (CH 3 CO) 2 O 5.9 Sodium sulfate, Na 2 SO 4 , anhydrous Weigh portions of 2 g of sodium sulfate into test tubes with polytetrafluoroethylene (PTFE)-lined caps. D
34、ry the test tubes at 500 C 20 C for 4 h 30 min without caps. Place them in a desiccator and let them cool. When cooled put on the caps and store the tubes at room temperature. Sodium sulfate can also be dried in larger portions and stored in a desiccator after cooling. Weigh portions of 2 g into tub
35、es when needed. 5.10 2,4,6-tribromophenol, C 6 H 2 Br 3 OH, (internal standard), CAS 118-79-6 5.11 Chlorophenols (standards) 2,3-dichlorophenol, C 6 H 3 Cl 2 OH, CAS 576-24-9 2,4-dichlorophenol, C 6 H 3 Cl 2 OH, CAS 120-83-2 2,5-dichlorophenol, C 6 H 3 Cl 2 OH, CAS 583-78-8 2,6-dichlorophenol, C 6 H
36、 3 Cl 2 OH, CAS 87-65-0 3,4-dichlorophenol, C 6 H 3 Cl 2 OH, CAS 95-77-2 3,5-dichlorophenol, C 6 H 3 Cl 2 OH, CAS 591-35-5 2,3,4-trichlorophenol, C 6 H 2 Cl 3 OH, CAS 15950-66-0 BSISO14154:2005IS:45141 O5002(E) I SO 5002 All irthgs ersedevr 3 2,3,5-trichlorophenol, C 6 H 2 Cl 3 OH, CAS 933-78-8 2,3,
37、6-trichlorophenol, C 6 H 2 Cl 3 OH, CAS 933-75-7 2,4,5-trichlorophenol, C 6 H 2 Cl 3 OH, CAS 95-95-4 2,4,6-trichlorophenol, C 6 H 2 Cl 3 OH, CAS 88-06-2 3,4,5-trichlorophenol, C 6 H 2 Cl 3 OH, CAS 609-19-8 2,3,4,5-tetrachlorophenol, C 6 HCl 4 OH, CAS 4901-51-3 2,3,4,6-tetrachlorophenol, C 6 HCl 4 OH
38、, CAS 58-90-2 Pentachlorophenol, C 6 Cl 5 OH, CAS 87-86-5 5.12 Sodium hydroxide solution, NaOH, c(NaOH) = 0,1 mol/l 5.13 Sodium hydroxide solution, NaOH, c(NaOH) = 0,5 mol/l 5.14 Potassium carbonate solution, K 2 CO 3 , c(K 2 CO 3 ) = 0,1 mol/l 5.15 Potassium carbonate solution, K 2 CO 3 , c(K 2 CO
39、3 ) = 5,2 mol/l 5.16 Internal standard solutions 5.16.1 Stock solution Prepare the stock solution of the internal standard by weighing 2,4,6-tribromophenol (5.10) and dissolving it in ethanol (5.2). A suitable concentration is given in Table A.1. Divide the stock solution into 5 ml bottles with tigh
40、t caps, 1,5 ml in each bottle, and store at 18 C. Stock solutions are stable for at least half a year when stored in the dark at 4 C. They are stable at least one year when stored at 18 C. NOTE 2,4-dibromophenol or 2,6-dibromophenol can also be used as internal standard. 5.16.2 Working solution Prep
41、are the working solution by diluting the stock solution (5.16.1) with water (5.1), and add a few drops of sodium hydroxide solution (5.13) to prevent precipitation. A suitable concentration of the internal standard working solution is given in Table A.1. 5.17 Standard solutions (see Table A.2) 5.17.
42、1 Stock solutions Weigh out each of the chlorophenol standards (5.11) into the same or into separate measuring flasks and dissolve them in ethanol (5.2). Divide the stock solution(s) into 5 ml bottles with tight PTFE-lined caps, 1,5 ml in each bottle, and store at 18 C. 5.17.2 Working solutions Dilu
43、te stock solution(s) (5.17.1) with distilled water to obtain a working solution, and add a few drops of sodium hydroxide solution (5.13) to prevent precipitation. 5.18 Acetone-hexane solution, 1:1 (volume fraction) BSISO14154:2005IS:45141 O5002(E) 4 I SO 5002 All irthgs ersedevr6 Apparatus Ordinary
44、laboratory apparatus and the following. 6.1 Standard laboratory glassware, appropriately cleaned and free of interfering compounds. Do not use any kind of plastics containers, since the chlorophenols may adsorb to these; plastics materials may also contribute their impurities to the sample material.
45、 6.2 Capillary gas chromatograph, preferably equipped with two electron-capture detectors and with the facility to connect two capillary columns to the same injection system or with two different injectors. Results achieved with single-column GC-ECD systems should be confirmed by additional GC-ECD a
46、nalysis using another column of different polarity or by GC-MS analysis. 6.3 Capillary columns, at least two, with stationary phases of different polarity. 6.4 Ultrasonic bath. 7 Sampling WARNING Soil contaminated with commercial mixtures of chlorophenols often contains impurities of polychlorinated
47、 phenoxyphenols (PCPPs), polychlorinated dibenzo-p-dioxins and dibenzofurans, and polychlorinated biphenyls (PCBs) in minor concentrations. There is thus a contamination risk in the laboratory. Take samples in accordance with ISO 10381-1 and pretreat the samples in accordance with ISO 14507. Place t
48、he samples in glass bottles with PTFE caps. It is recommended to fill the bottles completely. Store the samples in the dark in the laboratory either at 18 C or at +4 C. Chlorophenols can be subject to microbial conversion under certain conditions. It is recommended that samples be frozen if they are
49、 stored for more than 2 days. 8 Procedure 8.1 Test portion Using a spoon or a spatula, mix the field-moist soil as well as possible. Take a soil sample of at least 10 g, with an accuracy of 0,01 g, directly from the bottle. 8.2 Dry matter content Determine the dry matter content of the soil in a subsample from the same bottle in accordance with ISO 11465. 8.3 Blank sample Treat blank samples
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