《BS-EN-12673-1999 BS-6068-2.65-1999.pdf》由会员分享，可在线阅读，更多相关《BS-EN-12673-1999 BS-6068-2.65-1999.pdf（20页珍藏版）》请在三一文库上搜索。
1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS EN 12673:1999 BS 6068-
2、2.65: 1999 The European Standard EN 12673:1998 has the status of a British Standard ICS 13.060.50 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Water quality Gas chromatographic determination of some selected chlorophenols in water Licensed Copy: sheffieldun sheffieldun, na,
3、 Sat Oct 28 14:51:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI This British Standard, having been prepared under the direction of the Health and Environment Sector Committee, was published under the authority of the Standards Committee and comes into effect on 15 June 1999 BSI 06-1999 ISBN 0 580 30
4、998 3 BS EN 12673:1999 Amendments issued since publication Amd. No.DateComments National foreword This British Standard is the English language version of EN 12673:1998. The UK participation in its preparation was entrusted by Technical Committee EH/3, Water quality, to Subcommittee EH/3/2, Physical
5、, 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 interests informed; monitor related international and E
6、uropean 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 12673 is one of a series of standards on water quality, others of which have been, or will be, published as Sections of BS 6068. This standa
7、rd has therefore been given the secondary identifier BS 6068-2.65. The various Sections of BS 6068 are comprised within Parts 1 to 7, which, together with Part 0, are listed below. Part 0Introduction Part 1Glossary Part 2Physical, chemical and biochemical methods Part 3Radiological methods Part 4Mic
8、robiological methods Part 5Biological methods Part 6Sampling Part 7Precision and accuracy NOTEThe tests described in this British Standard should only be carried out by suitably qualified persons with an appropriate level of chemical expertise. Standard chemical procedures should be followed through
9、out. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled International Standards Correspondence Index, or by using the Find facility of the BSI Standards Elec
10、tronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users 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 d
11、ocument comprises a front cover, an inside front cover, the EN title page, pages 2 to 16, an inside back cover and a back cover. Licensed Copy: sheffieldun sheffieldun, na, Sat Oct 28 14:51:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI CEN European Committee for Standardization Comite Europe en de N
12、ormalisation Europa isches Komitee fu r Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1998 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 12673:1998 E EUROPEAN STANDARDEN 12673 NORME EUROPE ENNE EUROPA ISCHE NOR
13、M December 1998 ICS 13.060.01 Descriptors: water tests, water, quality, water pollution, chemical analysis, determination of content, phenols, chromatographic analysis, gas chromatography, extraction English version Water quality Gas chromatographic determination of some selected chlorophenols in wa
14、ter Qualite de leau Dosage par chromatographie en phase gazeuse de certains chlorophe nols dans les eaux Wasserbeschaffenheit Gaschromatographische Bestimmung einiger ausgewa hlter Chlorphenole in Wasser This European Standard was approved by CEN on 26 November 1998. CEN members are bound to comply
15、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 Central Secret
16、ariat 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 Central Secretariat has the same status as the offici
17、al versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. Licensed Copy: sheffieldun sheffieldun, na, Sa
18、t Oct 28 14:51:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 2 EN 12673:1998 BSI 06-1999 Foreword This European Standard has been prepared by Technical Committee CEN/TC 230, Water analysis, the Secretariat of which is held by DIN. This European Standard shall be given the status of a national s
19、tandard, either by publication of an identical text or by endorsement, at the latest by June 1999, and conflicting national standards shall be withdrawn at the latest by June 1999. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are
20、bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Annexes designated informative are only given for information
21、. In this standard annexes A to G are informative. It is absolutely essential that tests conducted according to this standard are carried out by suitably qualified staff. Licensed Copy: sheffieldun sheffieldun, na, Sat Oct 28 14:51:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 3 EN 12673:1998 B
22、SI 06-1999 1 Scope This European Standard describes the gas chromatographic determination of 19 chlorophenols (2-, 3-, and 4-chlorophenol, 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-trichlorophenol, 2,3,4,5-, 2,3,4,6-, and 2,3,5,6-tetrachloro
23、phenol and pentachlorophenol) in drinking water, groundwater, rainwater, waste water, sea water and surface water. This standard describes an acetylation followed by a liquid/liquid extraction and determination by gas chromatography and electron capture detection or mass selective detection. The met
24、hod is validated for drinking water, surface water and waste water, but may be used for all above mentioned types of water. With this method chlorophenols can be determined over a range of concentrations from 0,1 mg/l to 1 mg/l, depending on the quantity of sample used and the component sensitivity
25、(level of chlorination) (see annex A). In some cases complete separation of isomers cannot be achieved. Then the sum is reported. This method may be applicable to other halogenated phenolic compounds, provided the method is validated for each case. 2 Normative references This European Standard incor
26、porates by dated or undated reference, provisions from other publications. These normative references are cited at the appropriate places in the text and the publications are listed hereafter. For dated references subsequent amendments to or revisions of any of these publications apply to this Europ
27、ean Standard only when incorporated in it by amendment or revision. For undated references the latest edition of the publication referred to applies. ISO 5667-5:1991, Water quality Sampling Part 5: Guidance on sampling of drinking water and water used for food and beverage processing. ISO 5667-6:199
28、0, Water quality Sampling Part 6: Guidance on sampling of rivers and streams. ISO 5667-8:1993, Water quality Sampling Part 8: Guidance on sampling of wet deposition. ISO 5667-9:1992, Water quality Sampling Part 9: Guidance on sampling from marine waters. ISO 5667-10:1992, Water quality Sampling Part
29、 10: Guidance on sampling from waste waters. ISO 5667-11:1993, Water quality Sampling Part 11: Guidance on sampling from ground waters. 3 Definitions For the purpose of this European Standard the following definition applies. 3.1 chlorophenol compound having an aromatic nucleus carrying one hydroxyl
30、 group and from one to five chlorine atoms 4 Principle Chlorophenols present in the aqueous samples are derivatized with acetic anhydride to their corresponding acetates. The derivatives formed are extracted from the sample with hexane. The hexane fraction is analysed by gas chromatography with elec
31、tron capture detection or mass selective detection. Depending on the sample type pretreatment involves acid-base partition prior to the derivatization step. 5 Interferences Surfactants, emulsifiers, higher concentrations of polar solvents and other phenolic substances can affect the extractive deriv
32、atization step. Suspended particles in the water can also interfere and reduce the recovery. A second liquid phase in the water (e.g. mineral oil compounds, highly volatile halogenated hydrocarbons, emulsified fats and waxes) disturbs sampling, sample preparation and the enrichment. In those cases t
33、he examination is restricted to the aqueous phase and the portion of the non-aqueous phase is reported separately. 6 Reagents WARNING The use of this European Standard may involve hazardous materials, operations and equipment. This standard does not purport to address all the safety problems associa
34、ted with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 6.1 General requirements All reagents shall be of such a purity that they do not give rise to significa
35、nt interfering peaks in the gas chromatographic analysis of the extracts. This shall be verified for each batch of material by running procedural blanks with each batch of samples analyzed. Reagents shall be stored in all glass containers with glass stoppers or with polytetrafluoroethylene (PTFE) li
36、ned caps. 6.2 Gas chromatographic gases, including helium, argon/methane, nitrogen or hydrogen. They shall be of a purity as recommended by the gas chromatograph manufacturer. 6.3 Ethanol, C2H5OH. 6.4 n-Hexane, C6H14. 6.5 Potassium carbonate solution, c(K2CO3) = 1,0 mol/l. 6.6 Potassium carbonate so
37、lution, c(K2CO3) = 0,1 mol/l. 6.7 Acetic anhydride, C4H6O3. NOTEImpurities in the acetic anhydride may affect the recovery. In that case it is possible to purify acetic anhydride by distillation. Licensed Copy: sheffieldun sheffieldun, na, Sat Oct 28 14:51:09 GMT+00:00 2006, Uncontrolled Copy, (c) B
38、SI Page 4 EN 12673:1998 BSI 06-1999 6.8 Toluene, C7H8. 6.9 Phosphoric acid, c(H3PO4) = 0,5 mol/l. 6.10 Sodium sulfate, Na2SO4, anhydrous, neutral. NOTESome batches of sodium sulfate have been found to be alkaline. In these circumstances it is possible to wash with methanol containing 0,5 ml concentr
39、ated hydrochloric acid per litre and to dry on a steam bath before roasting in a muffle furnace (7.6) at 500 8C20 8C for 4 h0,5 h. 6.11 Sodium hydroxide, c(NaOH) = 0,1 mol/l. 6.12 Sodium thiosulfate pentahydrate, (Na2S2O35H2O), crystals or a 10 % (m/m) solution. 6.13 2-chlorophenol, C6H5OCl. 6.14 3-
40、chlorophenol, C6H5OCl. 6.15 4-chlorophenol, C6H5OCl. 6.16 2,3-dichlorophenol, C6H4OCl2. 6.17 2,4-dichlorophenol, C6H4OCl2. 6.18 2,5-dichlorophenol, C6H4OCl2. 6.19 2,6-dichlorophenol, C6H4OCl2. 6.20 3,4-dichlorophenol, C6H4OCl2. 6.21 3,5-dichlorophenol, C6H4OCl2. 6.22 2,3,4-trichlorophenol, C6H3OCl3.
41、 6.23 2,3,5-trichlorophenol, C6H3OCl3. 6.24 2,3,6-trichlorophenol, C6H3OCl3. 6.25 2,4,5-trichlorophenol, C6H3OCl3. 6.26 2,4,6-trichlorophenol, C6H3OCl3. 6.27 3,4,5-trichlorophenol, C6H3OCl3. 6.28 2,3,4,5-tetrachlorophenol, C6H2OCl4. 6.29 2,3,4,6-tetrachlorophenol, C6H2OCl4. 6.30 2,3,5,6-tetrachlorop
42、henol, C6H2OCl4. 6.31 Pentachlorophenol, C6Cl5OH. 6.32 Standard solutions of chlorophenols 6.32.1 Internal standard solutions Prepare solutions of at least two internal standards in ethanol (see 6.3). For electron capture detection the following internal standard can be used: 2,4-dibromophenol, C6H4
43、OBr2; 2,6-dibromophenol, C6H4OBr2; 2,3,6-trichlorophenol (see 6.24), C6H3OCl3; 2,4,6-tribromophenol, C6H3OBr3. For mass selective detection similar labelled compounds can be used. NOTEThe two internal standards are used as a control for the analytical procedure. The choice of the two internal standa
44、rds should reflect the anticipated occurrence of the chlorophenols in the sample (e.g. if dichlorophenols are expected 2,4-dibromophenol and 2,6-dibromophenol should be used). Prepare a mixed standard of two component solutions in such a concentration that if a small volume is added to a sample, the
45、 amount of the internal standards gives peak heights on the chromatogram in the upper part of the linear working range. Typically a concentration of 10 mg/ml can be used. Confirm their concentration prior to use. 6.32.2 Stock solutions Prepare stock solutions of the chlorophenols by weighing each co
46、mpound (6.13 to 6.31) and dissolving it in ethanol (6.3). Typical concentrations of the stock solutions are given in annex B. Alternatively, commercially available standard solutions can be used. Confirm the concentrations. NOTE 1Confirmation may be accomplished by spectrometric methods (e.g. UV spe
47、ctrometry) or comparison with a standard of known concentration or from another source. NOTE 2Stock solutions are stable for at least half a year when stored in the dark at 4 8C. At a temperature of 218 8C they are stable for at least one year. 6.32.3 Intermediate standards Prepare this mixed standa
48、rd solution by dilution of the stock solutions (6.32.2). Suitable concentrations are given in annex B. The intermediate standards should be prepared freshly every month. 6.32.4 Working standards Prepare a minimum of five different concentrations by suitable dilutions of the intermediate solution (6.
49、32.3) with ethanol (6.3). Suitable concentrations are given in annex B. The working standards may be used for 5 days. 7 Apparatus 7.1 General requirements Standard laboratory glassware cleaned to eliminate all interferences. NOTEHeating to a temperature above 150 8C before use assists in freeing glassware from possible contaminations. This procedure should not be used for volumetric bottles. Also an alkaline washing procedure can be used. 7.2 Sample bottles, all glass, with glass stoppers or with PTFE lined caps. A random