BS EN ISO 11732-2005 Water quality - Determination of ammonium nitrogen - Method by flow analysis (CFA and FIA) and spectrometric detection《水质 氨氮的测定 流动分析(CFA和FIA)和光谱测定法》.pdf

1、BRITISH STANDARD BS EN ISO 11732:2005 BS 6068-2.93:2005 Water quality Determination of ammonium nitrogen Method by flow analysis (CFA and FIA) and spectrometric detection The European Standard EN ISO 11732:2005 has the status of a British Standard ICS 13.060.50 BS EN ISO 11732:2005 This British Stan

2、dard was published under the authority of the Standards Policy and Strategy Committee on 17 February 2005 BSI 17 February 2005 ISBN 0 580 45490 8 National foreword This British Standard is the official English language version of EN ISO 11732:2005. It is identical with ISO 11732:2005. It supersedes

3、BS EN ISO 11732:1997 which is withdrawn. The UK participation in its preparation was entrusted by Technical Committee EH/3, Water quality, to Subcommittee EH/3/2, Physical, chemical and biochemical methods, which has the responsibility to: A list of organizations represented on this subcommittee can

4、 be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” f

5、acility 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 British Standard does not of itself confer immunity from legal obligat

6、ions. 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 European developments and promulgate them in the UK. Summary of

7、pages This document comprises a front cover, an inside front cover, the EN ISO title page, the EN ISO foreword page, the ISO title page, pages ii to v, a blank page, pages 1 to 18, an inside back cover and a back cover. The BSI copyright notice displayed in this document indicates when the document

8、was last issued. Amendments issued since publication Amd. No. Date Comments EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 11732 February 2005 ICS 13.060.50 Supersedes EN ISO 11732:1997 English version Water quality - Determination of ammonium nitrogen - Method by flow analysis (CFA and FI

9、A) and spectrometric detection (ISO 11732:2005) Qualit de leau - Dosage de lazote ammoniacal - Mthode par analyse en flux (CFA et FIA) et dtection spectromtrique (ISO 11732:2005) Wasserbeschaffenheit - Bestimmung von Ammoniumstickstoff - Verfahren mittels Flieanalytik (CFA und FIA) und spektrometris

10、cher Detektion (ISO 11732:2005) This European Standard was approved by CEN on 3 January 2005. 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-dat

11、e lists and bibliographical references concerning such national standards may be obtained on application to the Central Secretariat 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

12、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, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,

13、Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36

14、B-1050 Brussels 2005 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 11732:2005: E I NESO 11:2372005 (E) 2 Foreword This document (EN ISO 11732:2005) has been prepared by Technical Committee ISO/TC 147 “Water quality“ in collab

15、oration with 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 standard, either by publication of an identical text or by endorsement, at the latest by August 2005, and conflicting national standar

16、ds shall be withdrawn at the latest by August 2005. This document supersedes EN ISO 11732:1997. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic,

17、Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Endorsement notice The text of ISO 11732:2005 has been approved by CEN

18、 as EN ISO 11732:2005 without any modifications. ENISO11732:2005 Reference number ISO 11732:2005(E) OSI 5002INTERNATIONAL STANDARD ISO 11732 Second edition 2005-02-01 Water quality Determination of ammonium nitrogen Method by flow analysis (CFA and FIA) and spectrometric detection Qualit de leau Dos

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24、hi n Switlrez dnaii ISO 5002 Allr ithgsr esedevrENISO11732:2005IS:23711 O5002(E) I SO 5002 All irthgs ersedevr iiiContents Page Foreword iv Introduction v 1 Scope 1 2 Normative references . 1 3 Determination of ammonium nitrogen by flow injection analysis (FIA) and spectrometric detection 1 4 Determ

25、ination of ammonium nitrogen by continuous flow analysis (CFA) and spectrometric detection . 7 5 Calculation. 10 6 Precision 10 7 Test report . 11 Annex A (informative) Examples of flow analysis systems . 12 Annex B (informative) Precision data. 16 Bibliography . 18 ENISO11732:2005IS:23711 O5002(E)

26、iv I SO 5002 All irthgs ersedevrForeword 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 carried out through ISO technical committees. Each member body inter

27、ested 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. ISO collaborates closely with the International Electrotechnical

28、 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 International Standards. Draft International Standards adopted by the te

29、chnical 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 elements of this document may be the subject of patent rights. IS

30、O shall not be held responsible for identifying any or all such patent rights. ISO 11732 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical, chemical and biochemical methods. This second edition cancels and replaces the first edition (ISO 11732:1997), which ha

31、s been technically revised. ENISO11732:2005IS:23711 O5002(E) I SO 5002 All irthgs ersedevr vIntroduction Methods using flow analysis are automating wet chemical procedures and are therefore particularly suitable for the processing of large sample series at a high analysis frequency (up to 100 sample

32、s per hour). It is differentiated between flow injection analysis (FIA) 1,2and continuous flow analysis (CFA) 3 . Both methods consist of the automatic dosage of the sample introduced into a flow system (manifold) in which the sample analytes react with the reagent solutions on their way through the

33、 manifold. The sample preparation may be integrated into the manifold. The reaction product is measured in a flow detector. The user should be aware that particular problems could require the specification of additional marginal conditions. ENISO11732:2005blank 5002:23711OSINEINTENRATIONAL TSANDADR

34、IS:23711 O5002(E)I SO 5002 All irthgs ersedevr 1Water quality Determination of ammonium nitrogen Method by flow analysis (CFA and FIA) and spectrometric detection WARNING Persons using this International Standard should be familiar with normal laboratory practice. This International Standard does no

35、t purport 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. IMPORTANT It is absolutely essential that tests conducted acco

36、rding to this standard be carried out by suitably trained staff. 1 Scope This International Standard specifies methods suitable for the determination of ammonium nitrogen in various types of waters (such as ground, drinking, surface, and waste waters) in mass concentrations ranging from 0,1 mg/l to

37、10 mg/l (in the undiluted sample), applying either FIA (Clause 3) or CFA (Clause 4). In particular cases, the range of application may be adapted by varying the operating conditions. 2 Normative references The following referenced documents are indispensable for the application of this document. For

38、 dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 3696:1987, Water for analytical laboratory use Specification and test methods ISO 5667-1, Water quality Sampling Part 1: Guidance on the de

39、sign of sampling programmes ISO 5667-2, Water quality Sampling Part 2: Guidance on sampling techniques ISO 5667-3, Water quality Sampling Part 3: Guidance on the preservation and handling of water samples ISO 8466-1, Water quality Calibration and evaluation of analytical methods and estimation of pe

40、rformance characteristics Part 1: Statistical evaluation of the linear calibration function 3 Determination of ammonium nitrogen by flow injection analysis (FIA) and spectrometric detection 3.1 Principle The sample containing ammonium is injected into a continuous carrier stream by means of an injec

41、tion valve and is mixed with a continuously streaming flow of an alkaline solution. The ammonia formed is separated in a diffusion cell from the solution over a hydrophobic semipermeable membrane and taken up by a streaming recipient flow containing a pH indicator. Due to the resulting pH shift, the

42、 indicator solution will change its colour which is measured continuously in the flow photometer. Additional information about this analytical technique is given in references 4, 5, 6, 7 and 8. NOTE Equipment following this principle using CFA instead of FIA is commercially available, however it has

43、 not been validated. ENISO11732:2005IS:23711 O5002(E) 2 I SO 5002 All irthgs ersedevr3.2 Interferences Volatile amines, if present, diffuse through the membrane and lead to a pH shift. If the concentrations of the volatile amines (e.g. methylamine or ethylamine) are equal to those of the ammonium, h

44、igher results may then be expected 12 . Significant concentrations of volatile amines can be reduced by distilling the sample adjusted to pH 5,8 prior to the analysis. In rare cases, it may be possible that the sample does not reach a pH of 12 after the addition of the alkaline reagent solution, thu

45、s leading to a loss of ammonium because it will not be converted quantitatively into ammonia. This may particularly occur with strong acidic or buffered samples. In these cases, the pH of the sample shall be adjusted to the range of 3 to 5 by the addition of sodium hydroxide solution (3.3.2 or 3.3.3

46、). A high concentration of metal ions that can precipitate as hydroxides will give poorly reproducible results. The addition of a suitable complexing agent, such as ethylenedinitrilotetraacetic acid (EDTA), disodium salt, to the alkaline reaction solution (3.3.17) in sufficiently large concentration

47、 will prevent the interference by Cu, Zn, Fe, Ca, Mg, and Al. A concentration of 30 g/l of ethylenedinitrilotetraacetic acid, disodium salt (3.3.4), in solution R1 (3.3.17) is adequate for metal concentrations up to 0,2 mg/l each. In the case of samples containing particulate matter, see 3.5 (last p

48、aragraph). Samples with a total salt concentration of 10 g/l shall be diluted prior to the measurement. 3.3 Reagents Apart from the reagents dealt with in the 3.3.6 and 3.3.7, use only reagents of “analytical grade quality for the determination of nitrogen”, or, if not available, those of recognized

49、 “analytical grade quality”. The ammonium content of the blank shall regularly be checked (3.6.3). 3.3.1 Water, of grade 1 as specified in ISO 3696:1987. 3.3.2 Sodium hydroxide solution I, c(NaOH) = 5 mol/l. 3.3.3 Sodium hydroxide solution II, c(NaOH) = 0,01 mol/l. 3.3.4 Ethylenedinitrilotetraacetic acid (EDTA) 1) , disodium salt, monohydrate, C 10 H 14 N 2 Na 2 O 8 H 2 O. 3.3.5 Bromocresol