EN ISO 15681-1-2004 en Water quality - Determination of orthophosphate and total phosphorus contents by flow analysis (FIA and CFA) - Part 2 Method by continuous flow analysis (CFA.pdf

1、BRITISH STANDARD BS EN ISO 15681-1:2004 BS 6068-2.86:2004 Incorporating Corrigenda Nos. 1 and 2 and Amendment No. 1 to BS ISO 15681-1:2003 (Amendment No. 1 renumbers the BS ISO as BS EN ISO 15681-1:2004) Water quality Determination of orthophosphate and total phosphorus contents by flow analysis (FI

2、A and CFA) Part 1: Method by flow injection analysis (FIA) The European Standard EN ISO 15681-1:2004 has the status of a British Standard ICS 13.060.50 BS EN ISO 15681-1:2004 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 18 February 2004 BS

3、I 11 February 2005 ISBN 0 580 43182 7 National foreword This British Standard is the official English language version of EN ISO 15681-1:2004. It is identical with ISO 15681-1:2003. The UK participation in its preparation was entrusted by Technical Committee EH/3, Water quality, to Subcommittee EH/3

4、/2, Physical, chemical and biochemical methods, which has the responsibility to: A list of organizations represented on this subcommittee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this doc

5、ument may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the necessary provisions of a contract

6、. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for c

7、hange, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of 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

8、 page, pages 1 to 19 and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date Comments 15002 Corrigendum No. 1 18 February 2004 Addition of dual number on front cover and back cover 15545 7 Fe

9、bruary 2005 Implementation of the European Standard 15596 Corrigendum No. 2 11 February 2005 Replaced European pagesEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM ENISO156811 December2004 ICS13.060.50 Englishversion WaterqualityDeterminationoforthophosphateandtotal phosphoruscontentsbyflowanalysis(F

10、IAandCFA)Part1: Methodbyflowinjectionanalysis(FIA)(ISO156811:2003) QualitdeleauDosagedesorthophosphatesetdu phosphoretotalparanalyseenflux(FIAetCFA)Partie1: Mthodeparanalyseavecinjectionenflux(FIA)(ISO 156811:2003) WasserbeschaffenheitBestimmungvonOthophosphat undGesamtphosphormittelsFlieanalytik(FI

11、AundCFA) Teil1:VerfahrenmittelsFlieinjektionsanalyse(FIA)(ISO 156811:2003) ThisEuropeanStandardwasapprovedbyCENon21December2004. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.U

12、ptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheCentralSecretariatortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitso

13、wnlanguageandnotifiedtotheCentralSecretariathasthesamestatusast heofficial versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,Cyprus,CzechRepublic,Denmark,Estonia,Finland,France, Germany,Greece,Hungary,Iceland,Ireland,Italy,Latvia,Lithuania,Luxembourg,Malta,Netherlands,Norway,Poland,

14、Portugal, Slovakia, Slovenia,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2004CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembe

15、rs. Ref.No.ENISO156811:2004:E Foreword The text of ISO 15681-1:2003 has been prepared by Technical Committee ISO/TC 147 “Water quality” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 15681-1:2004 by Technical Committee CEN/TC 230 “Water analysis“, the s

16、ecretariat 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 June 2005, and conflicting national standards shall be withdrawn at the latest by June 2005. According to the CE

17、N/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg

18、, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Endorsement notice The text of ISO 15681-1:2003 has been approved by CEN as EN ISO 15681-1:2004 without any modifications. ENISO156811:2004 Reference number ISO 15681-1:2003(E)INTERNATI

19、ONAL STANDARD ISO 15681-1 First edition 2003-12-15 Water quality Determination of orthophosphate and total phosphorus contents by flow analysis (FIA and CFA) Part 1: Method by flow injection analysis (FIA) Qualit de leau Dosage des orthophosphates et du phosphore total par analyse en flux (FIA et CF

20、A) Partie 1: Mthode par analyse avec injection en flux (FIA) 3002:118651OSISBENISO156811:2004ISO 15681-1:2003(E) DPlcsid Fremia ihTs PDF file mya ctnoian emdebt dedyfepcaes. In ccacnadrow eitA hebods licnesilop gnic,y tihs file mirp eb yatnde iv roweb detu slahl ton ide ebtlnu deess teh typfecaes wi

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25、ISO156811:2004 iiiContents Page Foreword iv Introduction v 1 Scope 1 2 Normative references. 1 3 Interferences 2 3.1 General interferences. 2 3.2 Interferences in the determination of total-P . 2 4 Principle. 2 4.1 Determination of orthophosphate . 2 4.2 Total phosphorus with manual digestion. 2 5 R

26、eagents 2 6 Apparatus. 6 6.1 Flow injection analysis (FIA) 6 6.2 Additional apparatus 6 6.3 Additional apparatus for the determination of total phosphorus 6 7 Sampling and sample preparation 7 8 Procedure. 7 8.1 Analysis preparation. 7 8.2 Instrument performance check. 7 8.3 Reagent blank check 7 8.

27、4 Calibration 8 8.5 Check of digestion efficiency for determination of total-P. 8 8.6 Measurement. 8 8.7 Closing down the system. 8 9 Calculation of results 9 10 Expression of results 9 11 Test report 9 Annex A (informative) Example of an FIA system. 10 Annex B (informative) Precision and accuracy .

28、 11 Annex C (informative) Determination of orthophosphate-P and total-P by FIA using ascorbic acid reduction 13 Annex D (informative) Replacement of hydrazine sulfate by DEHA (N,N-diethylhydroxylamine) . 18 Bibliography . 19 3002:118651OSISBENISO156811:2004iv Foreword ISO (the International Organiza

29、tion 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 has been established

30、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 electrotechnical standardization. In

31、ternational 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 technical committees are circulated to the member bodies for voting. Publi

32、cation 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. ISO shall not be held responsible for identifying any or all such patent r

33、ights. ISO 15681-1 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical, chemical and biochemical methods. ISO 15681 consists of the following parts, under the general title Water quality Determination of orthophosphate and total phosphorus contents by flow anal

34、ysis (FIA and CFA): Part 1: Method by flow injection analysis (FIA) Part 2: Method by continuous flow analysis (CFA) BSISO13002:11865ENISO156811:2004 vIntroduction Methods of determining water quality using flow analysis automated wet chemical procedures, and are particularly suitable for the proces

35、sing of many analytes in water in large sample series at a high analysis frequency. Analysis can be performed by flow injection analysis (FIA) 1, 2or continuous flow analysis (CFA)3 . Both methods share the feature of an automatic dosage of the sample into a flow system (manifold) where the analyte

36、in the sample reacts with the reagent solutions on its way through the manifold. The sample preparation may be integrated in the manifold. The amount of reaction product is measured in a flow detector (e.g. flow photometer). This part of ISO 15681 describes the FIA method. The user should be aware t

37、hat particular problems could require the specification of additional marginal conditions. 3002:118651OSISBENISO156811:2004blank ENISO156811:2004INTENRATIONAL TSANDADR IS-18651 O1:(3002E)1Water quality Determination of orthophosphate and total phosphorus contents by flow analysis (FIA and CFA) Part

38、1: Method by flow injection analysis (FIA) WARNING Persons using this part of ISO 15681 should be familiar with normal laboratory practice. This part of ISO 15681 does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establis

39、h appropriate safety and health practices and to ensure compliance with any national regulatory conditions. Molybdate and antimony waste solutions should be disposed of properly. It is absolutely essential that tests conducted according to this part of ISO 15681 be carried out by suitably qualified

40、staff. 1 Scope This part of ISO 15681 specifies flow injection analysis (FIA) methods for the determination of orthophosphate in the mass concentration range from 0,01 mg/l to 1,0 mg/l (P), and total phosphorus by manual digestion in accordance with ISO 6878 5, 6for the mass concentration range from

41、 0,1 mg/l to 10 mg/l (P). The range of application can be changed by varying the operating conditions. This part of ISO 15681 is applicable to various types of water (such as ground, drinking, surface, leachate and waste waters). This method is also applicable to the analysis of seawater, but with c

42、hanges in sensitivity, by adaptation of the carrier and calibration solutions to the salinity of the samples. 2 Normative references The following reference documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references,

43、 the latest edition of the referenced document (including any amendments) applies. ISO 3696, Water for analytical laboratory use Specification and test methods ISO 5667-1, Water quality Sampling Part 1: Guidance on the design on sampling programmes ISO 5667-2, Water quality Sampling Part 2: Guidance

44、 on sampling techniques ISO 5667-3, Water quality Sampling Part 3: Guidance on the preservation and handling of water samples ISO 6878:1) , Water quality Determination of phosphorus Ammonium molybdate spectrometric method ISO 8466-1, Water quality Calibration and evaluation of analytical methods and

45、 estimation of performance characteristics Part 1: Statistical evaluation of the linear calibration function 1) To be published. 3002:118651OSISBENISO156811:20042 3 Interferences 3.1 General interferences ISO 6878:, Annex B gives a list of general interferences. In addition, or contrary to the cited

46、 standard, the following guidelines apply. a) Arsenate causes serious interference. 100 g/l As, present as arsenate, results in a response comparable to approximately 30 g/l P. b) If the silicate concentration in samples is not greater than 60 times the phosphorus concentration, interferences by sil

47、icate can be neglected. c) Fluoride interference is significant above 50 mg/l. d) Nitrite interference is significant above 5 mg/l. The interference can be eliminated by acidifying samples after collection. e) For samples containing high concentrations of oxidizing agents, the amount of added reduci

48、ng reagent can be insufficient. In this case it is advisable to remove the oxidizing material prior to digestion. f) The self-absorption of the sample can be compensated by measuring, in addition to the sample signal (8.6), the signal of the sample without the admixture of the reagents. In this case, the difference of the two responses is used for the evaluation (see Clause 9). 3.2 Interferences in the determination