1、BRITISH STANDARD BS EN ISO 10301:1997 BS 6068-2.58: 1997 Water quality Determination of highly volatile halogenated hydrocarbons Gas-chromatographic methods The European Standard EN ISO 10301:1997 has the status of a British Standard ICS 13.060.01BS EN ISO 10301:1997 This British Standard, having be
2、en prepared under the directionof the Health and Environment Sector Board, waspublished under the authorityof the StandardsBoardand comesintoeffecton 15July 1997 BSI 10-1999 ISBN 0 580 27541 8 Amendments issued since publication Amd. No. Date CommentsBSENISO10301:1997 BSI 10-1999 i Contents Page Nat
3、ional foreword ii Foreword 2 Foreword iv Text of ISO 10301 1BS EN ISO 10301:1997 ii BSI 10-1999 National foreword This British Standard is the English language version of EN ISO 10301:1997. It is identical with ISO 10301:1997. The UK participation in its preparation was entrusted by Technical Commit
4、teeEH/3, Water quality, to SubcommitteeEH/3/2, Physical, chemical and biochemical methods, which has the responsibility to: 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
5、interests informed; monitor related international and European developments and promulgate them in the UK. A list of organizations represented on this subcommittee can be obtained on request to its secretary. BS EN ISO 10301 is one of a series of standards on water quality, others of which have been
6、, or will be, published as Sections of BS6068. This standard has therefore been given the secondary identifier BS6068-2.58. The various Sections of BS6068 comprise Parts1 to7, which, together with Part0, are listed below. Part 0: Introduction; Part 1: Glossary; Part 2: Physical, chemical and biochem
7、ical methods; Part 3: Radiological methods; Part 4: Microbiological methods; Part 5: Biological methods; Part 6: Sampling; Part 7: Precision and accuracy. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BS
8、I Standards Catalogue under the section entitled “International Standards Correspondence Index”, or using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsib
9、le for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, theENISO title page, page 2, the ISO title page, pages ii to iv, pages 1 to 2
10、9 andaback cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM ENISO10301 April 1997 ICS 13.060.30 Descriptors: See ISO document
11、English version Water quality Determination of highly volatile halogenated hydrocarbons Gas-chromatographic methods (ISO10301:1997) Qualit de leau Dosage des hydrocarbures halogns hautement volatils Mthodes par chromatographie en phase gazeuse (ISO10301:1997) Wasserbeschaffenheit Bestimmung leichtfl
12、chtiger halogenierter Kohlenwasserstoffe Gaschromatographische Verfahren (ISO 10301:1997) This European Standard was approved by CEN on 1997-03-28. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of
13、 a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the Central Secretariat or to any CEN member. The European Standards exist in three official versions (English, French, German). A version
14、 in any other language made by translation under the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Denmark, Finland, France, Germany, Greece
15、, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1997 CEN ALL rights o
16、f exploitation in any form and by any means reserved worldwide for CENnational Members. Ref. No. EN ISO 10301:1997 E EN ISO 10301:1997 BSI 10-1999 2 Foreword The text of the International Standard ISO10301:1997 has been prepared by TechnicalCommittee ISO/TC 147 “Water quality” in collaboration with
17、Technical Committee CEN/TC230 “Water analysis”, the secretariat of which is held by DIN. 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 October1997, and conflicting national standards shall be wi
18、thdrawn at the latest by October1997. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Ne
19、therlands, Norway, Portugal, Spain, Sweden, Switzerland and the UnitedKingdom. Endorsement notice The text of the International Standard ISO10301:1997 was approved by CEN as a European Standard without any modification.ENISO10301:1997 ii BSI 10-1999 Contents Page Foreword iv Introduction 1 Section 1
20、. General 1.1 Scope 1 1.2 Normative references 2 1.3 Definition 2 Section 2. Liquid/liquid extraction and analysis by gas chromatography 2.1 Principle 3 2.2 Interferences 3 2.3 Reagents 3 2.4 Apparatus 4 2.5 Sampling and sample preparation 4 2.6 Procedure 5 2.7 Calibration 6 2.8 Identification and e
21、valuation 8 2.9 Expression of results 10 2.10 Precision data 10 2.11 Test report 11 Section 3. Static headspace method and analysis by gas chromatography 3.1 Principle 12 3.2 Interferences 12 3.3 Reagents 12 3.4 Apparatus 12 3.5 Sampling 12 3.6 Procedure 13 3.7 Calibration 13 3.8 Identification and
22、evaluation 15 3.9 Expression of results 16 3.10 Precision data 16 3.11 Test report 17 Annex A (informative) Characteristics of highly volatile halogenated hydrocarbons 18 Annex B (informative) Examples of gas chromatograms for highly volatile halogenated hydrocarbons 23 Annex C (informative) Example
23、 of a microseparator 27 Annex D (informative) Sensitivity of electron-capture detector 28 Annex E (informative) Extraction recovery with pentane 28 Annex F (informative) Qualitative method for testing the quality of “penicillin type” stoppers 29 Annex G (informative) Collection of samples 29 Figure
24、B.1 Chromatograms of standards simultaneously injected on two capillary columns 24 Figure B.2 Example of gas chromatogram of highly volatile halogenated hydrocarbons 26 Figure C.1 Microseparator 27 Table 1 Typical values of “quantification limits” for some highly volatile halogenated hydrocarbons us
25、ing liquid/liquid extraction 1 Table 2 Typical values of “quantification limits” for some highly volatile halogenated hydrocarbons using static head-space method 1 Table 3 Explanation of the subscripts used in the symbols 6 Table 4 Standard deviations of tap water 10ENISO10301:1997 BSI 10-1999 iii P
26、age Table 5 Precision data for drinking water 10 Table 6 Precision data for waste water 11 Table 7 Precision data for drinking water 16 Table 8 Precision data for waste water 17 Table D.1 Relative sensitivity of the electron-capture detector, related to chlorobenzene = 100 % (guide values) 28 Table
27、E.1 Example of extraction recovery with pentane from drinking water 28 Descriptors: Water, quality, water pollution, water tests, chemical analysis, determination of content, halohydrocarbons, gas phase chromatography. EN ISO 10301:1997 iv BSI 10-1999 Foreword ISO (the International Organization for
28、 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 established has the
29、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 standardization. Draft Inte
30、rnational Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least75% of the member bodies casting a vote. International Standard ISO10301 was prepared by Technical Committee ISO/TC147, Water
31、quality, Subcommittee SC2, Physical, chemical and biochemical methods. Annex A toAnnex G of this International Standard are for information only. ENISO10301:1997 BSI 10-1999 1 Section 1. General Introduction Highly volatile halogenated hydrocarbons are used in industrial, commercial and domestic fie
32、lds, and can enter a water body via waste water and may consequently contaminate drinking water. Furthermore, they can originate from the use of chlorine as an oxidizing agent in water and waste-water treatment. They also can be introduced by inappropriate handling. In addition, they can be formed b
33、y decomposition of higher molecular mass organohalogen derivatives. In uncontaminated ground water and rain water, the concentrations of halogenated hydrocarbons are generally below0,14g/l. In surface water they may be higher, depending on the origin and quality of the water. In untreated waste wate
34、r the concentrations may reach saturation of the aqueous phase. In general, the solubility of these compounds in organic solvents and in fatty material exceeds their solubility in water. 1.1 Scope This International Standard specifies two methods for the determination of highly volatile halogenated
35、hydrocarbons using gas chromatography. Section 2 specifies a method for the determination by liquid/liquid extraction of highly volatile halogenated hydrocarbons in drinking water, ground water, swimming pool water, most rivers and lakes and many sewage and industrial effluents. Typical values of “q
36、uantification limits” are given inTable 1. Table 1 Typical values of “quantification limits” for some highly volatile halogenatedhydrocarbons using liquid/liquid extraction Section 3 specifies a method for the determination of highly volatile halogenated hydrocarbons in drinking water, surface water
37、s and ground water by a static head-space method. Typical values of “quantification limits” are given inTable 2. In practise, the head-space method is applicable for industrial effluents as a screening method, but in some cases it is necessary to confirm the result by the liquid-liquid extraction me
38、thod. NOTEWhen applying this International Standard, the guideon analytical quality control for water analysis (see ISO/TR13530) should be followed, especially for the calibration steps. Table 2 Typical values of “quantification limits” for some highly volatile halogenated hydrocarbons using static
39、head-space method Compound Quantification limits 4g/l Dichloromethane 50 Chloroform 0,05 0,3 Carbon tetrachloride 0,01 0,1 1,1-Dichloroethane 1,0 5 1,2-Dichloroethane 5 10 1,1,1-Trichloroethane 0,02 0,1 1,1,2,2-Tetrachloroethane 0,05 0,1 Hexachloroethane 0,01 0,05 cis-1,2-Dichloroethylene 5 50 trans
40、-1,2-Dichloroethylene 1 10 Trichloroethylene 0,05 0,1 Tetrachloroethylene 0,1 Hexachlorobutadiene 0,01 Tribromomethane 0,1 1,1,2-Trichlorotrifluoroethane 0,1 Compound Quantification limits 4g/l Dichloromethane 50 Chloroform 0,3 Carbon tetrachloride 0,1 1,1-Dichloroethane 100 1,2-Dichloroethane 100 1
41、,1,1-Trichloroethane 0,1 1,1,2-Trichloroethane 20 1,1-Dichloroethylene 10 cis-1,2-Dichloroethylene 50 trans-1,2-Dichloroethylene 25 Trichloroethylene 0,2 Tetrachloroethylene 0,2 1,2-Dichloropropane 50 1,3-Dichloropropane 200 cis+trans-1,3-Dichloropropylene 10 Dibromomethane 0,3 Tribromomethane (Brom
42、oform) 5 1,2-Dibromoethane 2 Bromochloromethane 1 Bromodichloromethane 0,2 Dibromochloromethane 0,3 1,1,3-Trifluoroethane 1 EN ISO 10301:1997 2 BSI 10-1999 1.2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this Interna
43、tional Standard. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below. M
44、embers of IEC and ISO maintain registers of currently valid International Standards. ISO 5667-1:1980, Water quality Sampling Part1: Guidance on the design of sampling programmes. ISO 5667-2:1991, Water quality Sampling Part2: Guidance on sampling techniques. ISO/TR 13530:, Water quality Guide to ana
45、lytical quality control for water analysis 1) . 1.3 Definition For the purposes of this International Standard, the following definition applies: 1.3.1 highly volatile halogenated hydrocarbons fluorinated, chlorinated, brominated and/or iodinated mainly nonaromatic hydrocarbons composed of one to si
46、x atoms of carbon NOTETheir boiling points generally fall within the range of20 C to220 C at atmospheric pressure (seeAnnex A). 1) In preparation. ENISO10301:1997 BSI 10-1999 3 Section 2. Liquid/liquid extraction and analysis by gas chromatography 2.1 Principle The highly volatile halogenated hydroc
47、arbons are extracted into an organic solvent. The solution is then analysed by gas chromatography with an electron-capture detector or any other suitable detector. 2.2 Interferences Interferences can be due to the sampling procedure, vials and stoppers, solvents, gases, organic compounds in the labo
48、ratory atmosphere and contamination from the autosampler. Procedures for minimizing contamination are given in2.5 and2.6. 2.3 Reagents All reagents shall be of sufficient purity so as to not give rise to significant interfering peaks in the gas chromatogram of the solvent extract. The purity of reag
49、ents shall be verified by a suitable procedure, for example, by blank determinations (see2.6.4). Reagents can become contaminated by contact with air and other materials, particularly plastics, or by degradation caused by the action of light. Store all reagents in the dark in tightly sealed all-glass containers or other suitable vessels. 2.3.1 Water for the preparation of calibration solutions and blank The quality of the water used shall be determined. For e
