1、BS EN ISO23161:2011ICS 13.080.10NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDSoil quality Determination ofselected organotincompounds Gas-chromatographicmethodNational forewordThis British Standard is the UK implementation EN ISO 23161:2011. It is identical t
2、o ISO 23161:2009. It supersedes BS ISO 23161:2009, which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee EH/5, Sludge characterization.A list of organizations represented on this committee can be obtained on request to its secretary. BSI, as a member of CEN,
3、 is obliged to publish EN ISO 23161 as a British Standard. However, attention is drawn to the fact that the UK committee voted against its approval as a European Standard and has strong reservations about endorsing its publication as a British Standard. The UK committee believes that the reproducibi
4、lity obtained in interlaboratory evaluation was not an adequate basis on which to support a reference method to measure the concentration of an analyte (or analytes) in a sample within the scope of the method. This could cause problems in the event of dispute or litigation.The standard deviations of
5、 reproducibility in the interlaboratory validation trials of this method were poor and there is a low probability of getting the same result from two laboratories analysing the same sample. In the worst cases the standard deviation of reproducibility was about half the mean analysis (after rejection
6、 of outliers), for example agricultural soil mean 27,48 ngTPhT/g, SR14,33 ngTPhT/g; harbour sediment mean 3524,16 ngTBT/g, SR1018,88 ngTBT/g; and river sediment 219,72 ngMBT/g, SR135,27 ngMBT/g.BSI technical committee EH/5 advises caution in the application of this standard. If it is used in cases o
7、f dispute, analytical data should be reviewed carefully and preferably should be obtained from more than one laboratory.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application.Compliance with a British Standard cannot
8、 confer immunity from legal obligations.BS EN ISO 23161:2011This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 October 2009 BSI 2011ISBN 978 0 850 73259 1Amendments/corrigenda issued since publicationDate Comments30 November 2011 This corrige
9、ndum renumbers BS ISO 23161:2009 as BS EN ISO 23161:2011EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 23161 August 2011 ICS 13.080.10 English Version Soil quality - Determination of selected organotin compounds - Gas-chromatographic method (ISO 23161:2009) Qualit du sol - Dosage dune slec
10、tion de composs organostanniques - Mthode par chromatographie en phase gazeuse (ISO 23161:2009) Bodenbeschaffenheit - Bestimmung ausgewhlter Organozinnverbindungen - Gaschromatographisches Verfahren (ISO 23161:2009) This European Standard was approved by CEN on 14 July 2011. CEN members are bound to
11、 comply with the CEN/CENELEC 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 bibliographical references concerning such national standards may be obtained on application to the CEN-CE
12、NELEC 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 a CEN member into its own language and notified to the CEN-CENELEC Management Centre has t
13、he same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Pola
14、nd, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2011 CEN All rights of exploitation in any form and by a
15、ny means reserved worldwide for CEN national Members. Ref. No. EN ISO 23161:2011: EForeword The text of ISO 23161:2009 has been prepared by Technical Committee ISO/TC 190 “Soil quality” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 23161:2011 by Techni
16、cal Committee CEN/TC 308 “Characterization of sludges” the secretariat of which is held by AFNOR. 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 by February 2012, and conflicting national standards
17、shall be withdrawn at the latest by February 2012. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. According to the CEN/CENELEC Intern
18、al Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembo
19、urg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 23161:2009 has been approved by CEN as a EN ISO 23161:2011 without any modification. ii BS EN ISO 23161:2011EN ISO 23161:2011 (E) ISO
20、2011 iiiContents Page Foreword iv Introduction.v 1 Scope1 2 Normative references2 3 Terms and definitions .2 4 Principle2 5 Reagents.4 5.1 General .4 5.2 Chemicals.4 5.3 Standards .5 5.4 Preparation of reagents and solutions6 5.5 Clean-up .7 6 Apparatus.7 6.1 Requirements for glassware 7 6.2 Samplin
21、g apparatus 8 6.3 Additional apparatus.8 7 Procedure.8 7.1 Sampling and sample pretreatment 8 7.2 Sample extraction9 7.3 Clean-up of the extract10 7.4 Determination of dry mass .11 7.5 Measurement .11 8 Calibration12 9 Recovery rates of the internal standard compounds 12 10 Quantification 13 11 Expr
22、ession of results14 12 Precision.14 13 Test report14 Annex A (informative) Information about the procedure 15 Annex B (informative) Additional clean-up procedures17 Annex C (informative) Information about typical instrumental conditions20 Annex D (informative) Information about GC/MS identification.
23、31 Annex E (informative) Validation data 33 Bibliography37 BS EN ISO 23161:2011EN ISO 23161:2011 (E) ISO 2011 iv Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards
24、 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. International organizations, governmental and non-governmental, in liaison with ISO, also take p
25、art in the work. ISO collaborates closely with the International Electrotechnical Commission (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
26、 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 approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility t
27、hat 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 23161 was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical methods and soil characteristics. BS EN
28、ISO 23161:2011EN ISO 23161:2011 (E) ISO 2011 vIntroduction It is absolutely essential that tests conducted in accordance with this International Standard be carried out by suitably qualified staff. It can be noted whether, and to what extent, particular problems will require the specification of add
29、itional boundary conditions. BS EN ISO 23161:2011EN ISO 23161:2011 (E) ISO 2011 INTERNATIONAL STANDARD 1Soil quality Determination of selected organotin compounds Gas-chromatographic method WARNING Persons using this International Standard should be familiar with normal laboratory practice. This Int
30、ernational 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. 1 Scope This International Standard
31、 specifies a gas-chromatographic method for the identification and quantification of organotin compounds (OTCs) in soils as specified in Table 1. The method is also applicable to samples from sediments, sludges and wastes (soil-like materials). The working range depends on the detection technique us
32、ed and the amount of sample taken for analysis. The limit of quantification for each compound is about 10 g/kg. Table 1 Organotin compound, which can be determined in accordance with this International Standard RnSn(4n)+R n Name Acronym Organotin cationsaBuSn3+Butyl 1 Monobutyltin cation MBT Bu2Sn2+
33、Butyl 2 Dibutyltin cation DBT Bu3Sn+Butyl 3 Tributyltin cation TBT OcSn3+Octyl 1 Monooctyltin cation MOT Oc2Sn2+Octyl 2 Dioctyltin cation DOT Ph3Sn+Phenyl 3 Triphenyltin cation TPhT Cy3Sn+Cyclohexyl 3 Tricyclohexyltin cation TCyT Peralkylated organotin Bu4Sn Butyl 4 Tetrabutyltin TTBT aOrganotin com
34、pounds are measured after derivatization. NOTE When applying this method to the determination of other organotin compounds not specified in the scope, its suitability is proven by proper in-house validation experiments, e.g. methyltin compounds. See Table 2. Methyltin cations are unlikely to evapora
35、te from aqueous solvents, but peralkylated methyltin compounds are volatile and subject to losses (see C.3). Therefore, additional precautions are established. Table 2 Methyltin compounds RnSn(4n)+R n Name Acronym MeSn3+Methyl 1 Monomethyltin cation MMT Me2Sn2+Methyl 2 Dimethyltin cation DMT Me3Sn+M
36、ethyl 3 Trimethyltin cation TMT BS EN ISO 23161:2011 ISO 2011EN ISO 23161:2011 (E)2 Organotin cations can only be determined in accordance with this International Standard after derivatization. The anionic part bound to the organotin cation is mainly dependent on the chemical environment and is not
37、determined using this method. The peralkylated organotin compounds behave in a completely different way from their parent compounds. Tetraalkylated organotin compounds which are already peralkylated, such as tetrabutyltin, are determined directly without derivatization. The properties, such as parti
38、cle size distribution, water content and organic matter content of the solids to be analysed using this International Standard vary widely. Sample pretreatment is designed adequately with respect to both the properties of the organotin compounds and the matrix to be analysed. 2 Normative references
39、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 amendments) applies. ISO 3696, Water for analytical laboratory use Spe
40、cification and test methods ISO 11465, Soil quality Determination of dry matter and water content on a mass basis Gravimetric method ISO 16720, Soil quality Pretreatment of samples by freeze-drying for subsequent analysis ISO 22892, Soil quality Guidelines for the identification of target compounds
41、by gas chromatography and mass spectrometry 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 organotin compound substance containing 1 to 4 Sn-C bonds NOTE The number of Sn-C bonds is a measure for the degree of substitution. 3.2 organotin cat
42、ion part of the organotin compound (3.1) that contains all Sn-C bonds and is formally charged 3.3 organotin cation derivatives non-dissociated tetrasubstituted organotin compounds which are produced by derivatization 3.4 solid soil, sediment, sludge and waste (soil-like material) 4 Principle For the
43、 ionic and the non-ionic organotin compounds (see Table 1), a different sample pretreatment and sample preparation are necessary. For the determination of organotin cations, laboratory samples are pretreated by freeze drying and grinding. This procedure enables homogeneity of the sample to be achiev
44、ed. The determination of non-ionic TTBT cannot be carried out with freeze-dried materials due to evaporation losses, thus, it shall be determined in the field-moist sample. Organotin cations can only be determined after derivatization, whereas TTBT is already peralkylated and can be determined witho
45、ut derivatization (see the flowchart in Figure 1). BS EN ISO 23161:2011EN ISO 23161:2011 (E) ISO 2011 3Figure 1 Flowchart for the pretreatment and analysis of selected organotin compounds For the determination of organotin compounds, two alternative extraction methods are given, both followed by in
46、situ derivatization with a tetraethylborate compound and simultaneous extraction with hexane: a) treatment with acetic acid; b) treatment with methanolic potassium hydroxide. NOTE 1 If it is necessary to take a large amount of sample, extraction and derivatization can be done in two steps. An aliquo
47、t of the extract can be taken for derivatization. This also applies for samples with high levels of OTC contamination. NOTE 2 During in situ derivatization, the solid phase is still present. This supports the extraction by continuous changing of the polar organotin cations to the non-polar organotin
48、 cation derivates. In situ methods can improve the extraction efficiency, particularly for monoalkylated organotin compounds. NOTE 3 Other extraction techniques can be applied if a comparable extraction efficiency is achieved. BS EN ISO 23161:2011EN ISO 23161:2011 (E) ISO 2011 4 NOTE 4 Treatment with potassium hydroxide provides some degree of digestion and is recommended
