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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 13.060.01 Licensed Copy: sheffieldun sheffieldun, na, Sat Nov
2、18 01:47:57 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 10301:1997 This British Standard, having been prepared under the direction of the Health and Environment Sector Board, was published under the authority of the Standards Board and comes into effect on 15 July 1997 BSI 10-1999 ISBN 0 58
3、0 27541 8 Amendments issued since publication Amd. No.DateComments Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:47:57 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 10301:1997 BSI 10-1999i Contents Page National forewordii Foreword2 Forewordiv Text of ISO 103011 Licensed Copy: she
4、ffieldun sheffieldun, na, Sat Nov 18 01:47:57 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 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
5、entrusted by Technical Committee EH/3, Water quality, to Subcommittee EH/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 proposa
6、ls for change, and keep the UK 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 qua
7、lity, others of which have been, or will be, published as Sections of BS 6068. This standard has therefore been given the secondary identifier BS 6068-2.58. The various Sections of BS 6068 comprise Parts 1 to 7, which, together with Part 0, are listed below. Part 0: Introduction; Part 1: Glossary; P
8、art 2: Physical, chemical and biochemical 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
9、 this document may be found in the BSI 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. Use
10、rs of British Standards are responsible 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, the EN ISO title page, page 2, the ISO t
11、itle page, pages ii to iv, pages 1 to 29 and a back 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. Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:47:57 GMT+00:00
12、2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 10301 April 1997 ICS 13.060.30 Descriptors: See ISO document English version Water quality Determination of highly volatile halogenated hydrocarbons Gas-chromatographic methods (ISO 10301:1997) Qualit de leau D
13、osage des hydrocarbures halogns hautement volatils Mthodes par chromatographie en phase gazeuse (ISO 10301:1997) Wasserbeschaffenheit Bestimmung leichtflchtiger halogenierter Kohlenwasserstoffe Gaschromatographische Verfahren (ISO 10301:1997) This European Standard was approved by CEN on 1997-03-28.
14、 CEN members are bound to 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
15、application to the Central Secretariat or to any CEN member. The European Standards exist 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 Central Secretariat h
16、as the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. CEN European Committee for Sta
17、ndardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1997 CEN ALL rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 10301:1997 E Licensed Copy: sheffieldun sh
18、effieldun, na, Sat Nov 18 01:47:57 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 10301:1997 BSI 10-1999 2 Foreword The text of the International Standard ISO 10301:1997 has been prepared by Technical Committee ISO/TC 147 “Water quality” in collaboration with Technical Committee CEN/TC 230 “Water
19、 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 October 1997, and conflicting national standards shall be withdrawn at the latest by October 19
20、97. 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, Netherlands, Norway, Portugal, Spain
21、, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of the International Standard ISO 10301:1997 was approved by CEN as a European Standard without any modification. Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:47:57 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Licen
22、sed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:47:57 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 10301:1997 ii BSI 10-1999 Contents Page Forewordiv Introduction1 Section 1. General 1.1Scope1 1.2Normative references2 1.3Definition2 Section 2. Liquid/liquid extraction and analysis by gas c
23、hromatography 2.1Principle3 2.2Interferences3 2.3Reagents3 2.4Apparatus4 2.5Sampling and sample preparation4 2.6Procedure5 2.7Calibration6 2.8Identification and evaluation8 2.9Expression of results10 2.10Precision data10 2.11Test report11 Section 3. Static headspace method and analysis by gas chroma
24、tography 3.1Principle12 3.2Interferences12 3.3Reagents12 3.4Apparatus12 3.5Sampling12 3.6Procedure13 3.7Calibration13 3.8Identification and evaluation15 3.9Expression of results16 3.10Precision data16 3.11Test report17 Annex A (informative) Characteristics of highly volatile halogenated hydrocarbons
25、18 Annex B (informative) Examples of gas chromatograms for highly volatile halogenated hydrocarbons23 Annex C (informative) Example of a microseparator27 Annex D (informative) Sensitivity of electron-capture detector28 Annex E (informative) Extraction recovery with pentane28 Annex F (informative) Qu
26、alitative method for testing the quality of “penicillin type” stoppers29 Annex G (informative) Collection of samples29 Figure B.1 Chromatograms of standards simultaneously injected on two capillary columns24 Figure B.2 Example of gas chromatogram of highly volatile halogenated hydrocarbons26 Figure
27、C.1 Microseparator27 Table 1 Typical values of “quantification limits” for some highly volatile halogenated hydrocarbons using liquid/liquid extraction1 Table 2 Typical values of “quantification limits” for some highly volatile halogenated hydrocarbons using static head-space method1 Table 3 Explana
28、tion of the subscripts used in the symbols6 Table 4 Standard deviations of tap water10 Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:47:57 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 10301:1997 BSI 10-1999iii Page Table 5 Precision data for drinking water10 Table 6 Precision data f
29、or waste water11 Table 7 Precision data for drinking water16 Table 8 Precision data for waste water17 Table D.1 Relative sensitivity of the electron-capture detector, related to chlorobenzene = 100 % (guide values)28 Table E.1 Example of extraction recovery with pentane from drinking water28 Descrip
30、tors: Water, quality, water pollution, water tests, chemical analysis, determination of content, halohydrocarbons, gas phase chromatography. Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:47:57 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 10301:1997 iv BSI 10-1999 Foreword ISO (the I
31、nternational 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 subject for which a technical committee
32、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 Commission (IEC) on all matters of electrotechnica
33、l standardization. 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. International Standard ISO 10301 was prepared by Techn
34、ical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical, chemical and biochemical methods. Annex A to Annex G of this International Standard are for information only. Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:47:57 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 10301
35、:1997 BSI 10-19991 Section 1. General Introduction Highly volatile halogenated hydrocarbons are used in industrial, commercial and domestic fields, 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
36、an oxidizing agent in water and waste-water treatment. They also can be introduced by inappropriate handling. In addition, they can be formed by decomposition of higher molecular mass organohalogen derivatives. In uncontaminated ground water and rain water, the concentrations of halogenated hydrocar
37、bons are generally below 0,1 4g/l. In surface water they may be higher, depending on the origin and quality of the water. In untreated waste water the concentrations may reach saturation of the aqueous phase. In general, the solubility of these compounds in organic solvents and in fatty material exc
38、eeds their solubility in water. 1.1 Scope This International Standard specifies two methods for the determination of highly volatile halogenated hydrocarbons using gas chromatography. Section 2 specifies a method for the determination by liquid/liquid extraction of highly volatile halogenated hydroc
39、arbons in drinking water, ground water, swimming pool water, most rivers and lakes and many sewage and industrial effluents. Typical values of “quantification limits” are given in Table 1. Table 1 Typical values of “quantification limits” for some highly volatile halogenated hydrocarbons using liqui
40、d/liquid extraction Section 3 specifies a method for the determination of highly volatile halogenated hydrocarbons in drinking water, surface waters and ground water by a static head-space method. Typical values of “quantification limits” are given in Table 2. In practise, the head-space method is a
41、pplicable for industrial effluents as a screening method, but in some cases it is necessary to confirm the result by the liquid-liquid extraction method. NOTEWhen applying this International Standard, the guide on analytical quality control for water analysis (see ISO/TR 13530) should be followed, e
42、specially for the calibration steps. Table 2 Typical values of “quantification limits” for some highly volatile halogenated hydrocarbons using static head-space method CompoundQuantification limits 4g/l Dichloromethane50 Chloroform0,05 0,3 Carbon tetrachloride0,01 0,1 1,1-Dichloroethane1,0 5 1,2-Dic
43、hloroethane5 10 1,1,1-Trichloroethane0,02 0,1 1,1,2,2-Tetrachloroethane0,05 0,1 Hexachloroethane0,01 0,05 cis-1,2-Dichloroethylene5 50 trans-1,2-Dichloroethylene1 10 Trichloroethylene0,05 0,1 Tetrachloroethylene0,1 Hexachlorobutadiene0,01 Tribromomethane0,1 1,1,2-Trichlorotrifluoroethane 0,1 Compoun
44、dQuantification limits 4g/l Dichloromethane50 Chloroform0,3 Carbon tetrachloride0,1 1,1-Dichloroethane100 1,2-Dichloroethane100 1,1,1-Trichloroethane0,1 1,1,2-Trichloroethane20 1,1-Dichloroethylene10 cis-1,2-Dichloroethylene50 trans-1,2-Dichloroethylene25 Trichloroethylene0,2 Tetrachloroethylene0,2
45、1,2-Dichloropropane50 1,3-Dichloropropane200 cis+trans-1,3-Dichloropropylene10 Dibromomethane0,3 Tribromomethane (Bromoform)5 1,2-Dibromoethane2 Bromochloromethane1 Bromodichloromethane0,2 Dibromochloromethane0,3 1,1,3-Trifluoroethane1 Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:47:57
46、GMT+00:00 2006, Uncontrolled Copy, (c) BSI 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 International Standard. At the time of publication, the editions indicated were valid. A
47、ll 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. Members of IEC and ISO maintain registers of currently valid International Standar
48、ds. ISO 5667-1:1980, Water quality Sampling Part 1: Guidance on the design of sampling programmes. ISO 5667-2:1991, Water quality Sampling Part 2: Guidance on sampling techniques. ISO/TR 13530:, Water quality Guide to analytical quality control for water analysis1). 1.3 Definition For the purposes o
49、f 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 six atoms of carbon NOTETheir boiling points generally fall within the range of 20 C to 220 C at atmospheric pressure (see Annex A). 1) In preparation. Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:47:57 GMT+00:00 2006, Uncontrolled Cop