BS EN ISO 14403-2-2012 Water quality Determination of total cyanide and free cyanide using flow analysis (FIA and CFA) Method using continuous flow analysis (CFA)《水质 连续流量分析测定总氰化物和游.pdf

1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN ISO 14403-2:2012Water quality Determinationof total cyanide and freecyanide using flow analysis(FIA and CFA)Part 2: Method using continuous flowanalysis (CFA) (ISO 14403-2:

2、2012)BS EN ISO 14403-2:2012 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO14403-2:2012. It supersedes BS EN ISO 14403:2002 which iswithdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee EH/3/2, Physical chemical and biochemica

3、l methods.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2012. Published by BS

4、I StandardsLimited 2012ISBN 978 0 580 66026 9ICS 13.060.50Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 31 July 2012.Amendments issued since publicationDate Text

5、 affectedEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 14403-2 July 2012 ICS 13.060.50 Supersedes EN ISO 14403:2002English Version Water quality - Determination of total cyanide and free cyanide using flow analysis (FIA and CFA) - Part 2: Method using continuous flow analysis (CFA) (ISO 1

6、4403-2:2012) Qualit de leau - Dosage des cyanures totaux et des cyanures libres par analyse en flux continu (FIA et CFA) - Partie 2: Mthode par analyse en flux continu (CFA) (ISO 14403-2:2012) Wasserbeschaffenheit - Bestimmung von Gesamtcyanid und freiem Cyanid mittels Flieanalytik (FIA und CFA) - T

7、eil2: Verfahren der kontinuierlichen Durchflussanalyse (CFA) (ISO 14403-2:2012) This European Standard was approved by CEN on 13 July 2012. 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 natio

8、nal standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A vers

9、ion in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, C

10、zech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom.

11、 EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 14403-2:2012: EBS E

12、N ISO 14403-2:2012EN ISO 14403-2:2012 (E) 3 Foreword This document (EN ISO 14403-2:2012) has been prepared by Technical Committee ISO/TC 147 “Water quality“ in collaboration with Technical Committee CEN/TC 230 “Water analysis” the secretariat of which is held by DIN. This European Standard shall be

13、given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by January 2013, and conflicting national standards shall be withdrawn at the latest by January 2013. Attention is drawn to the possibility that some of the elements of this document

14、may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes EN ISO 14403:2002. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are boun

15、d to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal

16、, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 14403-2:2012 has been approved by CEN as a EN ISO 14403-2:2012 without any modification. BS EN ISO 14403-2:2012ISO 14403-2:2012(E) ISO 2012 All rights reserved iiiContents Pag

17、eForeword ivIntroduction v1 Scope 12 Normative references . 13 Terms and definitions . 14 Interferences . 24.1 Interferences by oxidizing agents . 24.2 Interferences by sulfide, sulfite, nitrite and carbonyl compounds 24.3 Other interferences . 25 Principle . 35.1 Determination of total cyanide . 35

18、.2 Determination of free cyanide 36 Reagents 37 Apparatus 68 Sampling and sample preparation 89 Procedure 99.1 Flow system set-up . 99.2 Reagent blank measurement . 99.3 Checking the suitability of the flow system .109.4 Calibration .109.5 Sample measurement . 1110 Calculation 1111 Expression of res

19、ults . 1112 Test report . 11Annex A (informative) Examples of flow systems .13Annex B (normative) Determination of the real cyanide concentration in the potassium cyanide solution 16Annex C (informative) Example for the determination of total cyanide and free cyanide by continuous flow analysis (CFA

20、) with gas diffusion and amperometric detection .17Annex D (informative) Performance data .19Bibliography .21BS EN ISO 14403-2:2012ISO 14403-2:2012(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work

21、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 has the right to be represented on that committee. International organizations, governmental and non-government

22、al, 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.International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.The main

23、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. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote.Attent

24、ion 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 rights.ISO 14403-2 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical, chem

25、ical and biochemical methods.This first edition of ISO 14403-2 cancels and replaces ISO 14403:2002, which has been technically revised.ISO 14403 consists of the following parts, under the general title Water quality Determination of total cyanide and free cyanide using flow analysis (FIA and CFA): P

26、art 1: Method using flow injection analysis (FIA) Part 2: Method using continuous flow analysis (CFA)iv ISO 2012 All rights reservedBS EN ISO 14403-2:2012ISO 14403-2:2012(E)IntroductionMethods using flow analysis automate wet chemical procedures and are particularly suitable for the processing of ma

27、ny analytes in water in large series of samples at a high frequency of analysis.Analysis can be performed by flow injection analysis (FIA) or continuous flow analysis (CFA). Both methods share the feature of an automatic introduction of the sample into a flow system (manifold) in which the analytes

28、in the sample react with reagent solutions on their way through the manifold. Sample preparation may be integrated in the manifold. The reaction product is measured in a flow detector (e.g. flow photometer).See the foreword for a list of parts of this International Standard.It should be investigated

29、 whether and to what extent particular problems require the specification of additional marginal conditions. ISO 2012 All rights reserved vBS EN ISO 14403-2:2012BS EN ISO 14403-2:2012Water quality Determination of total cyanide and free cyanide using flow analysis (FIA and CFA) Part 2: Method using

30、continuous flow analysis (CFA)WARNING Persons using this part of ISO 14403 should be familiar with normal laboratory practice. This part of ISO 14403 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

31、 safety and health practices and to ensure compliance with any national regulatory conditions.IMPORTANT It is absolutely essential that tests conducted according to this part of ISO 14403 be carried out by suitably trained staff.1 ScopeThis part of ISO 14403 specifies methods for the determination o

32、f cyanide in various types of water (such as ground, drinking, surface, leachate, and waste water) with cyanide concentrations usually from 2 g/l to 500 g/l expressed as cyanide ions in the undiluted sample. The range of application can be changed by varying the operation conditions, e.g. by dilutin

33、g the original sample or changing the pathlength of the flow cell.In this method, a suitable mass concentration range from10 g/l to 100 g/l is described.Seawater can be analysed with possible changes in sensitivity and adaptation of the reagent and calibration solutions to the salinity of the sample

34、s.2 Normative referencesThe following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 3696, Water for analyt

35、ical and laboratory use Specification and test methods ISO 5667-3, Water quality Sampling Part 3: Preservation and handling of water samplesISO 8466-1, Water quality Calibration and evaluation of analytical methods and estimation of performance characteristics Part 1: Statistical evaluation of the l

36、inear calibration functionISO 8466-2, Water quality Calibration and evaluation of analytical methods and estimation of performance characteristics Part 2: Calibration strategy for non-linear second-order calibration functions3 Terms and definitionsFor the purpose of this part of ISO 14403, the follo

37、wing definitions apply:3.1free cyanideeasily liberatable cyanidesum of cyanide ions and the cyanide bound in weak metal cyanide complexes that liberate HCN at pH 3,8INTERNATIONAL STANDARD ISO 14403-2:2012(E) ISO 2012 All rights reserved 1BS EN ISO 14403-2:2012ISO 14403-2:2012(E)3.2total cyanidefree

38、cyanide (3.1), and in addition stronger metalcyanide complex compounds, with the exception of cyanide bound in gold, cobalt, platinum, ruthenium, and rhodium complexes, from which recovery can be partialNOTE 1 Thiocyanate, organically bound cyanide and cyanate are not included in this definition of

39、total cyanide.NOTE 2 Distillation methods may recover some organic cyanide. Use the diffusion method when organic cyanide complexes are suspected to be present.4 Interferences4.1 Interferences by oxidizing agentsOxidizing agents such as chlorine decompose most of the cyanides. If the presence of oxi

40、dizing agents cannot be excluded, treat the sample immediately after sampling. Test a drop of the sample with potassium iodide-starch test paper (KI starch paper); a blue colour indicates the need for treatment. Add sodium thiosulfate, a few crystals at a time, until a drop of sample produces no col

41、our on the indicator paper. Then add an additional portion of 0,6 g of ascorbic acid (6.9) for each 1 000 ml of sample volume.Do not add ascorbic acid unless samples will be analysed within 24 h.4.2 Interferences by sulfide, sulfite, nitrite and carbonyl compoundsInterferences by sulfide start at 10

42、0 mg/l. It affects the colorimetric procedure, especially the gas diffusion method, and the amperometric procedure (see Annex C). If a drop of the sample on lead acetate test paper indicates the presence of sulfide, treat an additional 25 ml of the stabilized sample (pH 12) to that required for the

43、cyanide determination with powdered lead carbonate.Lead sulfide precipitates if the sample contains sulfide.Repeat this operation until a drop of the treated sample solution does not darken the lead acetate test paper.Filter the solution through a dry filter paper into a dry beaker, and from the fil

44、trate measure the sample to be used for analysis. Avoid a large excess of lead and a long contact time in order to minimize loss by complexation or occlusion of cyanide on the precipitated material.If the amperometric method (Annex C) is applied, it is necessary systematically to add lead carbonate

45、to samples during the analysis (a few milligrams for a 10 ml sample), followed by filtration or decantation performed before the filtered sample aliquot is placed on the sample tray of the continuous flow analyser.Aldehydes and ketones can, under certain conditions, absorb cyanide by nucleophilic ad

46、dition. To avoid this interference ethylenediamine can be added to the sample.Under the given distillation conditions, aldehydes can transform cyanide to nitrite. Aldehydes can be removed by adding silver nitrate to the sample. The addition of AgNO3can alter the ratio of the concentrations of free a

47、nd total cyanide. The user should evaluate this procedure.Interference by nitrite above concentrations of 5 mg/l can be avoided by addition of sulfamic acid (6.10) to the buffer (pH 3,8) for the distillation and gas diffusion method (6.21.1).Sulfite interferes above concentrations of 1 mg/l.4.3 Othe

48、r interferencesSamples containing particulate matter can lead to losses if the particles clog the transport tubes and are not transported completely into the UV unit. This effect can be minimized by homogenizing (e.g. stirring) the sample immediately prior to analysis to ensure that a representative

49、 sample is taken and to reduce the particle size. Remaining particles with diameters 0,1 mm should be removed by filtration.2 ISO 2012 All rights reservedBS EN ISO 14403-2:2012ISO 14403-2:2012(E)When using in-line distillation for separation of the hydrogen cyanide, salt concentrations higher than 10 g/l of salts can cause clogging of the distillation coil. Dilute these samples prior to measurement or use a gas diffusion method in order to overcome this problem.Thiocyanate can slightly interfere and lead to positive bias (9.3.2).