1、BRITISH STANDARD BS ISO 14507:2003 Soil quality Pretreatment of samples for determination of organic contaminants ICS 13.080.01 BS ISO 14507:2003 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 11 April 2003 BSI 11 April 2003 ISBN 0 580 41554
2、 6 National foreword This British Standard reproduces verbatim ISO 14507:2003 and implements it as the UK national standard. The UK participation in its preparation was entrusted by Technical Committee EH/4, Soil quality, to Subcommittee EH/4/3, Chemical methods and soil characteristics, which has t
3、he 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 BSI Catalogue under the section entitled “Int
4、ernational 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 for its correct application. Compliance with a
5、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 interests informed; monitor related internationa
6、l 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 v, a blank page, page 1 to 14, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates
7、when the document was last issued. Amendments issued since publication Amd. No. Date Comments Reference number ISO 14507:2003(E)INTERNATIONAL STANDARD ISO 14507 First edition 2003-03-15 Soil quality Pretreatment of samples for determination of organic contaminants Qualit du sol Prtraitement des chan
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11、n to it is f,dnuo lpsaee inform ttneC ehlar Secrteiraat ta the serddaig sleb nevwo. ISO 3002 Athgir lls serevr.de selnUs towrehise specfidei, trap on fo thsi ilbupctanoi may cudorper ebtu ro dezilina ni dey fomr yb ro nam y,snae lecetrinoc ro mecinahcal, inclidung tohpcoiypodna gn micrfoilm, wittuoh
12、 repmissii non writign from eitI rehSa Ot tsserdda eh ebolw or ISOs memreb i ydobn the cnuotrfo y ttseuqer ehe.r ISO cirypothg fofice saCe tsopale 65 eneG 1121-HC 02 av leT. 4 + 10 947 22 1 11 xaF0 947 22 14 + 9 74 E-mail coirypthgiso.o gr We bwww.is.o gro Published in Switzerland ii BSISO14507:2003
13、 iiiContents Page Foreword iv Introduction v 1 Scope 1 2 Normative references . 1 3 Terms and definitions. 1 4 Principle . 2 4.1 Sampling 2 4.2 Volatile compounds 2 4.3 Moderately volatile compounds 2 5 Reagents 3 6 Apparatus 3 7 Preservation and storage. 4 8 Procedure 4 8.1 General. 4 8.2 Volatile
14、compounds (boiling point 300 C) Grinding necessary 5 8.4 Moderately volatile organic compounds (boiling point 300 C) Grinding not possible or not necessary . 7 8.5 Blank measurements 8 9 Test report . 8 Annex A (informative) Information concerning vapour pressure, boiling and melting points of volat
15、ile organic compounds 9 Annex B (informative) Validation 12 Bibliography . 14 BSISO14507:2003iv Foreword 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 carr
16、ied 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 part in the work.
17、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 prepare Internat
18、ional 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 that some of the e
19、lements 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 14507 was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical methods and soil characteristics. BSISO14507:2003 vIntrod
20、uction The properties of organic micropollutants can differ greatly according to chemical species: they can range from non-volatile to very volatile compounds (low to high vapour pressure); they can be labile or reactive at ambient or elevated temperatures; they can be biodegradable or UV-degradable
21、; they can have considerably different solubilities in water; they require different analytical procedures. Because of these differences, a general pretreatment procedure cannot be proposed. The goal of a pretreatment procedure is to prepare a test sample in which the concentration of the contaminan
22、t is equal to the concentration in the original soil, provided, however, that this procedure does not alter the chemical species to be analysed. For instance, if the sample contains only small particles and the contaminant is homogeneously distributed, it is not necessary to grind the sample. In thi
23、s International Standard, the size 2 mm is used to distinguish between small and large soil particles. Consistency among the following aspects is important: soil diversity; the aim of the analysis (including its accuracy); the nature of the chemical species to be analysed. The particle size distribu
24、tion of the sample in relation to the mass of sample taken for analysis is also important to pretreatment. For the analysis of organic contaminants, the sample mass taken in most cases is about 20 g. With such a sample mass, and provided that the contaminant is homogeneously distributed and the part
25、icles in the sample are smaller than about 2 mm, further grinding of the sample is not necessary. If the sample contains large particles or if the contaminant is heterogeneously distributed (as occurs for instance with tar particles), it is not possible to take a representative test sample of about
26、20 g without grinding the sample. To improve the homogeneity, samples are ground to a size smaller than 1 mm. Prior to analysis, very often no information about the distribution of the contaminant in the soil is known. Some analytical procedures start with a field-moist sample. Drying of the sample
27、gives lower extraction results. If the sample is not dried, grinding is not possible. In a situation in which accurate results are needed, the best available pretreatment procedure should be used. If it is necessary to establish whether the concentration is above a certain limit and it is already kn
28、own that the soil is heavily polluted, the simplest pretreatment procedure may meet the need. In this case however, the result may not be presented as a representative value for the whole sample. The choice depends above all on the volatility of the organic compounds under analysis. It also depends
29、on the soil particle size distribution, the heterogeneity of the sample and the analytical procedure. BSISO14507:2003INTENRATIONAL TSANDADR IS:70541 O3002(E)1Soil quality Pretreatment of samples for determination of organic contaminants 1 Scope This International Standard specifies three methods for
30、 the pretreatment of soil samples in the laboratory prior to the determination of organic contaminants: if volatile organic compounds are to be measured; if moderately volatile to non-volatile organic compounds are to be measured, if the result of the subsequent analysis must be accurate and reprodu
31、cible, and if the sample contains particles larger than 2 mm and/or the contaminant is heterogeneously distributed; if non-volatile organic compounds are to be measured and the extraction procedure prescribes a field- moist sample, or if the largest particles of the sample are smaller than 2 mm and
32、the contaminant is homogeneously distributed. This procedure is also applicable if reduced accuracy and repeatability are acceptable. The pretreatment described in this International Standard is used in combination with an extraction procedure in which the contaminant is available for the extraction
33、 liquid. NOTE For the pretreatment of soil samples for the purposes of determining non-volatile inorganic compounds and physico-chemical soil characteristics, see ISO 11464. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated re
34、ferences, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 10381-1, Soil quality Sampling Part 1: Guidance on the design of sampling programmes ISO 11074-2, Soil quality Vocabulary Part 2: Terms and definiti
35、ons relating to sampling ISO 11465:1993, Soil quality Determination of dry matter and water content on a mass basis Gravimetric method 3 Terms and definitions For the purposes of this document, the terms and definitions in ISO 11074-2 and the following apply: 3.1 volatile compound organic compound h
36、aving a boiling point below 300 C (at a pressure of 101 kPa) NOTE 1 This includes volatile aromatic and volatile halogenated hydrocarbons as determined in accordance with ISO 15009. Some mono- and dichlorophenols, for instance, and naphthalene also belong to this group. BSISO14507:20032 NOTE 2 The s
37、election of the categories for volatile and moderately volatile compounds can be related in principle to the vapour pressure. However, as the vapour pressure of only a small number of compounds is known, and in view of the relationship between vapour pressure and boiling point, the boiling point has
38、 been chosen as the criterion for distinction. See Annex A. 3.2 moderately volatile compound organic compound having a boiling point above 300 C (at a pressure of 101 kPa) NOTE 1 This definition includes: a) mineral oil (see ISO/TR 11046); b) most polycyclic aromatic hydrocarbons (PAH) (see ISO 1387
39、7); c) polychlorobiphenyls (PCB) (see ISO 10382); d) organochlorine pesticides (see ISO 10382). NOTE 2 In ISO/TR 11046, mineral oil is defined as the group of hydrocarbons which, on chromatography, have retention times lying between that of n-decane (C 10 H 22 ) and n-tetracontane (C 40 H 82 ). As i
40、n this International Standard the limit for volatile compounds lies at a boiling point of 300 C approximately hexadecane (C 16 ), this means that mineral oil should be considered as a volatile compound, as part of the compounds to be determined fall within the boiling point range of volatile compoun
41、ds. However for practical reasons, it has been decided that the pretreatment for moderately volatile compounds should be specified for the determination of mineral oil. As a result of cryogenic crushing, an improvement in the extraction yield occurs for compounds with a boiling point above 300 C. Th
42、e possible losses for the lower-boiling hydrocarbons (C 10to C 16 ) are assumed to be low, due to the retaining effect of the higher-boiling hydrocarbons present in mineral oil and to be compensated by the higher extraction yield of the other hydrocarbons present. As the total yield is used to deter
43、mine the mineral oil as a group parameter, it is assumed that pretreatment using the method for moderately volatile compounds gives the best results at present. 4 Principle 4.1 Sampling Sampling shall be carried out in accordance with ISO 10381-1. The samples taken shall be kept cool and processed a
44、s soon as possible. The method of pretreatment depends on the volatility of the organic compound(s) or group(s) of organic compounds to be determined. When taking a subsample, the quantity of soil should be removed from the sample container in such a way that this quantity: a) is a subsample over th
45、e full depth of the sample, and b) can be taken quickly. 4.2 Volatile compounds For determination of volatile organic compounds, core test samples are taken from the sample and extracted according to the relevant specific analytical procedure. If composite samples are required, extracts of individua
46、l samples are mixed. It is not possible to obtain composite samples without severe losses of volatiles. The procedure is described in 8.2. 4.3 Moderately volatile compounds Samples are chemically dried at a low temperature ( 196 C, liquid nitrogen). The dried samples are cooled with liquid nitrogen
47、and ground with a cross-beater mill with a sieve of 1 mm mesh size (cryogenic crushing). After grinding, suitable test portions are processed according to the relevant specific analytical procedures. Composite samples can be prepared by mixing the ground samples. This procedure is described in 8.3.
48、BSISO14507:2003 3If the extraction procedure requires a field-moist sample, drying and grinding are not possible. If the original sample only contains a small fraction of particles greater than 2 mm and the distribution of contaminants is likely to be homogeneous, grinding may be omitted. In these t
49、wo cases, suitable test portions are taken directly after mixing the sample. This procedure is described in 8.4. NOTE 1 To distinguish the volatile organic compounds from the moderately volatile organic compounds, boiling points are used instead of the vapour pressure at ambient temperature. This is explained in Annex A, which also gives boiling points and vapour pressures of compounds regularly determined in soil investigati
