DIN EN 14207-2003 Water quality - Determination of epichlorohydrin German version EN 14207 2003《水质 3-氯-1 2-环氧丙烷的测定》.pdf

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1、DEUTSCHE NORM September 2003 Water quality English version of DIN EN 14207 Determination of epichlorohydrin DIN EN 14207 ICs 13.060.50 Wasserbeschaffenheit - Bestimmung von Epichlorhydrin European Standard EN 14207 : 2003 has the status of a DIN Standard. A comma is used as the decimal marker. This

2、standard is part of the series Deutsche Einheitsverfahren zur Wasser-, Abwasser- und Schlamm- untersuchung - Einzelkomponenten (Gruppe P) (German standard methods for the examination of water, waste water and sludge - Individual constituents (group P). National foreword This standard has been prepar

3、ed by CEN/TC 230 Water analysis (Secretariat: Germany). The responsible German body involved in its preparation was the Normenausschuss Wasserwesen (Water Practice Standards Committee). Expert assistance and specialized laboratories will be required to perform the analysis described in this standard

4、. Depending on the objective of the analysis, a check shall be made on a case-by-case basis as to whether and to what extent additional conditions will have to be specified. Standard methods published as DIN Standards are obtainable from Beuth Verlag GmbH, either individually or grouped in volumes.

5、The standard methods included in the loose-leaf publication entitled Deutsche Einheitsverfahren zur Wasser-, Abwasser- und Schlammuntersuchung will continue to be published by Wiley-VCH Verlag and Beuth Verlag GmbH. Continued overleaf. EN comprises 17 pages. O No part of this standard may be reprodu

6、ced without the prior permission of DIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany, has the exclusive right of sale for German Standards (DIN-Normen). Ref. No. DIN EN 14207 : 2003-09 English price group 11 Sales No. 11 11 12.03 Page 2 DIN EN 14207 : 2003-09

7、 Standard methods or draft standards bearing the group title German standard methods for the examination of water, waste water and sludge are classified under the following categories (main titles): General information (group A) (DIN 38402) Sensory analysis (group B) (DIN 38403) Physical and physico

8、chemical parameters (group C) (DIN 38404) Anions (group D) (DIN 38405) Cations (group E) (DIN 38406) Substance group analysis (group F) (DIN 38407) Gaseous constituents (group G) (DIN 38408) Parameters characterizing effects and substances (group H) (DIN 38409) Biological-ecological methods of analy

9、sis (group M) (DIN 3841 O) Microbiological methods (group K) (DIN 3841 1) Test methods using water organisms (group L) (DIN 3841 2) Individual constituents (group P) (DIN 3841 3) Sludge and sediments (group S) (DIN 3841 4) Bio-assays with microorganisms (group T) (DIN 3841 5) In addition to the meth

10、ods described in the DIN 38402 to DIN 38415 series of standards, there are a number of European Standards available, which also form part of the collection of German standard methods. Information on Parts of these series of standards that have already been published can be obtained from the offices

11、of theNormenausschuss Wasserwesen, telephone (030) 2601 -2448, or from Beuth Verlag GmbH, Burg- grafenstrae 6, 10787 Berlin, Germany. EUROPEAN STANDARD EUROPISCHE NORM NORME EUROPENNE EN 14207 April 2003 ICs 13.060.50 English version Water quality Determination of epichlorohydrin Qualit de leau - Do

12、sage de Ipichlorhydrine Wasserbeschaffenheit - Bestimmung von Epic h I orh yd ri n This European Standard was approved by CEN on 2003-01 -1 7. CEN members are bound to comply with the CENKENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a nat

13、ional standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the Management Centre or to any CEN member. The European Standards exist in three official versions (English, French, German). A version in any

14、other language made by translation under the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, the Czech Republic, Denmark, Finland, France, Germa

15、ny, Greece, Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, the Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland, and the United Kingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Management Centre: rue de Stassar

16、t 36, B-1050 Brussels O 2003. CEN - All rights of exploitation in any form and by any means reserved worldwide for GEN national members. Ref. No. EN 14207 : 2003 E Page 2 EN 14207 : 2003 Contents Page Foreword 3 Introduction . 3 1 Scope 3 2 Normative references 3 3 Principle 4 4 Interferences / Loss

17、es . 4 5 Reagents . 4 6 Apparatus . 6 7 Sampling . 7 8 Procedure . 7 9 Calibration 8 10 Calculation of the results 10 11 Expression of results 10 12 Test report 10 13 Precision data . 11 Annex A (informative) Example of sorbents . 12 Annex B (informative) Examples of recommended capillary columns 12

18、 Annex C (informative) Examples of chromatograms and spectra . 13 Page 3 EN 14207 : 2003 Foreword This document EN 14207:2003 has been prepared by Technical Committee CENTTC 230 “Water analysis”, the secretariat of which is held by DIN. This European Standard shall be given the status of a national

19、standard, either by publication of an identical text or by endorsement, at the latest by October 2003, and conflicting national standards shall be withdrawn at the latest by October 2003. Annexes A, B and C are informative. WARNING - Persons using this standard should be familiar with normal laborat

20、ory practice. This standard does not propose 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. According to the CENKENELEC

21、 Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard : Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Slov

22、akia, Spain, Sweden, Switzerland and the United Kingdom. Introduction It is highly recommended that the test described in this standard be carried out by suitably qualified staff. It should be investigated whether and to what extent particular problems will require the specification of additional ma

23、rginal conditions. 1 Scope This European Standard specifies a method for the determination of epichlorohydrin in drinking water and water used for drinking water processing. According to the given procedure, the limit of determination in routine analysis is about 0,5 pgh l). The limit of determinati

24、on can be lowered to monitor 0,l pg/l. 2 Normative references This European Standard incorporates 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 refere

25、nces, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incorporated in it by amendment or revision. For undated references the latest edition of the publication referred to applies (including amendments). EN 25667-1, Water quality - Samplin

26、g - Part 1: Guidance on the design of sampling programmes (IS0 5667- 1:1980). EN 25667-2, Water quality - Sampling - Part 2: Guidance on sampling techniques (IS0 5667-2: 1991). 1) This value was checked in an interlaboratory trial. Page 4 EN 14207 : 2003 EN IS0 5667-3, Water quality - Sampling - Par

27、t 3: Guidance on the preservation and handling of samples (IS0 5667-3: 1994). IS0 5667-5, Water quality - Sampling - Part 5: Guidance on sampling of drinking water and water used for food and beverage processing. IS0 8466-1, Water quality - Calibration and evaluation of analytical methods and estima

28、tion of performance characteristics - Part I: Statistical evaluation of the linear calibration function. 3 Principle Solid phase extraction of epichlorohydrin from the drinking water sample followed by gas chromatography using a mass spectrometer (MS) as detector. Alternatively, an electron capture

29、detector (ECD) can be used. 4 Interferences / Losses 4.1 Interferences during sampling In order to avoid interferences, withdraw the sample according to clause 7, taking into account the information given in EN 25667-1, EN 25667-2 and EN IS0 5667-3. In order to avoid losses due to the easy decomposi

30、tion of epichlorohydrin, avoid unnecessary storage and analyse the sample as soon as possible after sampling. If storage is unavoidable, store between 2 “C and 5 “C until sample pretreatment. 4.2 Interferences during enrichment The commercially available adsorbance materials are often of varying qua

31、lity. Considerable batch-to-batch differences in quality and selectivity of these materials are possible. Perform calibration and analysis with one and the same batch of material. Make sure to avoid any losses when removing the residual water in the adsorbance material (8.1.2). 4.3 Interferences in

32、the gas chromatography and mass spectrometry Set the operational conditions in accordance with the manufacturers instructions. Check these settings at regular intervals. General interferences, caused by the injection system can be eliminated with the help of special laboratory experience and the ins

33、truments manuals. The stability of the analytical system should be checked (for example by application of a measuring standard). 5 Reagents Use reagents of the reagent grade “for residual analysis” or equivalent as far as available. Impurities in the reagents and in the water contributing to the bla

34、nk shall be negligibly low. Check the blank regularly, especially prior to the use of a new batch. 5.1 Water Use double-distilled water or water of comparable purity. Page 5 EN 14207 : 2003 5.2 Operating gases for the gas chromatography / mass spectrometry / ECD, according to the manufacturers instr

35、uctions. The operating gases shall be of high purity. 5.3 Nitrogen, high purity, minimum 99,996 % (v/v), for removal of water in the sorbent packing after sample extraction. 5.4 Solvents 5.4.1 Diisopropyl ether, C6HI40. 5.4.2 Methanol, CHJOH, as conditioning agent. 5.5 Reducing agents, e.g. sodium t

36、hiosulfate (Na2S203). 5.6 Epichlorohydrin stock solution Weigh 50 mg of epichlorohydrin (C3H5CIO) into a 100-ml volumetric flask containing diisopropyl ether (5.4.1) up to the neck and fill to mark with diisopropyl ether (5.4.1). Store the solution in a refrigerator between 2 “C and 5 OC. The shelf-

37、life of the solution is limited (about 6 months). Check the concentration prior to analysis in order to make sure that no significant differences arise. 5.7 Internal standard stock solution The internal standard shall not be present in the sample itself. 5.7.1 3C3-epichlorohydrin stock solution for

38、GC-MS This solution may be purchased as certified solution (e.g. at a concentration of 100 pg/ml in nonane) or prepared from pure standard material according to 5.6. Never add more than 100 pI of a diluted internal standard stock solution in diisopropyl ether (5.4.1) to 100 ml of the water sample, a

39、 greater volume may result in poor recovery. NOTE The peak area of the internal standard should be equivalent to that of 1 pgA of the analyte. For example, if the con- centration of the stock solution is 100 pg/ml of 13C3-epichlorohydrin in nonane, 100 pI, dissolved in 1 ml diisopropyl ether (5.4.1)

40、 is required to produce a 10 pg/ml spiking solution from which a volume of 10 pI can be injected directly into 100 ml of water (5.1). 5.7.2 Ethyl 2-chloropropionate (C5H9C102) stock solution for GC-ECD (see 5.6) 5.8 Epichlorohydrin spiking solutions Using stock standard solution (5.6), prepare spiki

41、ng solutions by appropriate dilution in a 100-ml volumetric flask containing diisopropyl ether (5.4.1). Prepare the spiking solutions at concentrations such that the aqueous calibration solutions (5.9) will cover the working range of the analytical system. Store spiking solutions in a refrigerator b

42、etween 2 OC and 5 OC. Let the solutions adjust to room temperature before preparing calibration solutions. The storage time shall not exceed one month. 5.9 Epichlorohydrin calibration solutions for the multipoint calibration Prepare aqueous calibration solutions from the spiking solutions (5.8) by i

43、njection of an appropriate volume (e.g. 10 pi) of the spiking solution directly into 100 ml of water (5.1). However, do not use more than 100 pl of a spiking solution to produce the calibration solutions. Mix the aqueous calibration solutions thoroughly by inverting the flask several times. Prepare

44、five different concentration levels. Prepare calibration solutions fresh daily. Table 1 gives an example for a dilution scheme. Page 6 EN 14207 : 2003 Millilitre of 5.6 added to 100 ml 5.4.1 02 Analyte concentration in the spiking solution in milligram per millilitre Concentration (in microgram per

45、litre) in the calibration solution ( 10 pl of the spiking solution added to 100 ml water ) 0,001 O, 1 If the desired measuring range differs from that of Table 1, different solution ratios should be taken. 5.10 Solid phase material Solid phase material on styrene-divinylbenzene copolymer basis is no

46、rmally used, e.g. commercially available cartridges or adequately glass columns filled with a minimum packing of 200 mg of the sorbent (see annex A). A recovery of 2 80 % of the analyte is required. 6 Apparatus 6.1 General requirements Equipment or parts of it which may come into contact with the wa

47、ter sample or the extract should be free from interfering compounds. 6.2 Sample bottles, preferably brown glass, 500 ml, with glass stoppers or PTFE-lined (PTFE = polytetrafluoro- ethene) screw caps. 6.3 Solid phase extraction cartridges, see 5.10. 6.4 Vacuum or pressure assembly, for the extraction

48、 step. 6.5 Volumetric flasks with inert stopper. 6.6 Vials, suitable for automatic or manual injection, preferably brown glass, with PTFE-lined septa. 6.7 Capillary gas chromatograph, equipped with a mass spectrometer as detector or an ECD. Preferably use an autosampler for sample injection. For ope

49、rational aspects of the instruments the manufacturers instructions should be followed. 6.8 Capillary injector, for split-splitless, cold on-column or programmed temperature vaporizing (PTV) injection. 6.9 Capillary columns for gas chromatography, examples see annex B. 6.10 Injection syringes, nominal capacity 5 pI or 10 pl. Page 7 EN 14207 : 2003 7 Sampling Collect samples according to EN 25667-1, EN 25667-2, EN IS0 5667-3, and IS0 5667-5. Use for sampling carefully cleaned, preferably brown glass bottles, 500 ml . Fill the bottles completely with the water to be examined.