BS EN ISO 15681-2-2004 Water quality - Determination of orthophosphate and total phosphorus contents by flow analysis (FIA and CFA) - Method by continuous flow analysis (CFA)《水质 用流.pdf

1、BRITISH STANDARD BS EN ISO 15681-2:2004 BS 6068-2.87: 2004 Incorporating Corrigenda Nos. 1 and 2 and Amendment No. 1 to BS ISO 15681-2:2003 (Amendment No. 1 renumbers the BS ISO as BS EN ISO 15681-2:2004) Water quality Determination of orthophosphate and total phosphorus contents by flow analysis (F

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

3、BSI 8 March 2005 ISBN 0 580 43181 9 National foreword This British Standard is the official English language version of EN ISO 15681-2:2004. It is identical with ISO 15681-2:2003. The UK participation in its preparation was entrusted by Technical Committee EH/3, Water quality, to Subcommittee EH/3/2

4、, 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 docum

5、ent 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 cha

7、nge, 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 p

8、age, pages 1 to 16, an inside back cover 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 15003 Corrigendum No. 1 18 February 2004 Correction to dual numbering on front cover

9、and back cover 15546 28 February 2005 Implementation of the European Standard 15625 Corrigendum No. 2 8 March 2005 Replaced European pagesEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM ENISO156812 December2004 ICS13.060.50 Englishversion WaterqualityDeterminationoforthophosphateandtotal phosphorusco

10、ntentsbyflowanalysis(FIAandCFA)Part2: Methodbycontinuousflowanalysis(CFA)(ISO156812:2003) QualitdeleauDosagedesorthophosphatesetdu phosphoretotalparanalyseenflux(FIAetCFA)Partie2: Mthodeparanalyseenfluxcontinu(CFA)(ISO15681 2:2003) WasserbeschaffenheitBestimmungvonOthophosphat undGesamtphosphormitte

11、lsFlieanalytik(FIAundCFA) Teil2:VerfahrenmittelskontinuierlicherDurchflussanalyse (CFA)(ISO156812:2003) ThisEuropeanStandardwasapprovedbyCENon21December2004. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationals

12、tandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheCentralSecretariatortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertherespo

13、nsibilityofaCENmemberintoitsownlanguageandnotifiedtotheCentralSecretariathasthesamestatusast heofficial versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,Cyprus,CzechRepublic,Denmark,Estonia,Finland,France, Germany,Greece,Hungary,Iceland,Ireland,Italy,Latvia,Lithuania,Luxembourg,Mal

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

15、 worldwideforCENnationalMembers. Ref.No.ENISO156812:2004:E Foreword The text of ISO 15681-2:2003 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 15681-2:2004 by Technical Committee CEN/T

16、C 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 June 2005, and conflicting national standards shall be withdrawn at the latest by J

17、une 2005. 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, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy,

18、Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Endorsement notice The text of ISO 15681-2:2003 has been approved by CEN as EN ISO 15681-2:2004 without any modifications. ENISO156812:2004 Reference number

19、 ISO 15681-2:2003(E)INTERNATIONAL STANDARD ISO 15681-2 First edition 2003-12-15 Water quality Determination of orthophosphate and total phosphorus contents by flow analysis (FIA and CFA) Part 2: Method by continuous flow analysis (CFA) Qualit de leau Dosage des orthophosphates et du phosphore total

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23、. In tlnu ehikletneve y ttah lborp aem lertait gno it is f,dnuo plsaee ifnrom ttneC ehlar Secterirata ta teh serddaig sleb nevwo. ii 3002:218651OSISBENISO156812:2004 iiiContents Page Foreword iv Introduction v 1 Scope 1 2 Normative references. 1 3 Interferences 2 3.1 General interferences. 2 3.2 Int

24、erferences in the determination of total-P . 2 4 Principle. 2 4.1 Determination of orthophosphate . 2 4.2 Total phosphorus with manual digestion. 3 4.3 Total phosphorus with integral UV digestion and hydrolysis 3 5 Reagents 3 6 Apparatus. 7 6.1 Continuous-flow analysis (CFA) 7 6.2 Additional apparat

25、us 7 6.3 Additional apparatus for the determination of total phosphorus after integral digestion 8 7 Sampling and sample preparation 8 8 Procedure. 8 8.1 Preparation for analysis . 8 8.2 Instrument performance check. 8 8.3 Reagent blank check 9 8.4 Calibration 9 8.5 Check of UV digestion and hydroly

26、sis for total P determination (see Figure A.2) 9 8.6 Measurement. 10 8.7 Closing down the system. 10 9 Calculation of results 10 10 Expression of results 10 11 Test report 10 Annex A (informative) Examples of a CFA system . 12 Annex B (informative) Precision and accuracy . 14 Annex C (informative) D

27、etermination of orthophosphate-P and total-P by CFA and tin(II) chloride reduction 15 Bibliography . 16 3002:218651OSISBENISO156812:2004iv Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of prepari

28、ng 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 has the right to be represented on that committee. International organizations, governmental and non-governmental, in lia

29、ison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical 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

30、technical committees is to prepare International Standards. 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. Attention is

31、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 rights. ISO 15681-2 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical, chemical a

32、nd biochemical methods. ISO 15681 consists of the following parts, under the general title Water quality Determination of orthophosphate and total phosphorus contents by flow analysis (FIA and CFA): Part 1: Method by flow injection analysis (FIA) Part 2: Method by continuous flow analysis (CFA) 3002

33、:218651OSISBENISO156812:2004 vIntroduction Methods of determining water quality using flow analysis automated wet chemical procedures and are particularly suitable for the processing of many analytes in water in large sample series at a high analysis frequency. Analysis can be performed by flow inje

34、ction 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 in the sample reacts with the reagent solutions on its way through the manifold. The sample preparation may be integrated

35、 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 CFA method. The user should be aware that particular problems could require the specification of additional marginal conditions. 3002:218651OSISBENISO156812:20

36、044002:218651OSINEINTENRATIONAL TSANDADR IS-18651 O2:(3002E)1Water quality Determination of orthophosphate and total phosphorus contents by flow analysis (FIA and CFA) Part 2: Method by continuous flow analysis (CFA) WARNING Persons using this part of ISO 15681 should be familiar with normal laborat

37、ory 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 establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions. Molybdate and anti

38、mony 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 staff. 1 Scope This part of ISO 15681 specifies CFA methods for the determination of orthophosphate in the mass concentration

39、range from 0,01 mg/l to 1,00 mg/l P, and total phosphorus in the mass concentration range from 0,10 mg/l to 10,0 mg/l P. The method includes the digestion of organic phosphorus compounds and the hydrolysis of inorganic polyphosphate compounds, performed either manually as described in ISO 6878 5, 6o

40、r with an integrated UV digestion and hydrolysis unit. This part of ISO 15681 is applicable to various types of water (such as ground, drinking, surface, leachate and waste water). The range of application may be changed by varying the operating conditions. This method is also applicable to the anal

41、ysis of seawater, but with changes in sensitivity, by adaptation of the carrier and calibration solutions to the salinity of the samples. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited app

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

43、lity 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 6878: 1) , Water quality Determination of phosphorus Ammonium molybdate spectrometric method 1) To be published. 3002:218651OSISBENISO156812

44、:20042 ISO 8466-1, Water quality Calibration and evaluation of analytical methods and estimation of performance characteristics Part 1: Statistical evaluation of the linear calibration function 3 Interferences 3.1 General interferences ISO 6878:, Annex B gives a list of general interferences. In add

45、ition, or contrary to the cited 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 conc

46、entration, interferences by silicate 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 age

47、nts, the amount of added reduction reagent can be insufficient. In this case, 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

48、. In this case, the difference of the two responses is used for the evaluation (Clause 9). 3.2 Interferences in the determination of total-P Samples containing solids or suspended particles can show low values when analysed by the UV method, if the particles are not completely transported into the UV unit. The error can be minimized by stirring the sample immediately before sampling, in order to ensure that a representati