DIN EN ISO 14403-2-2012 Water quality - Determination of total cyanide and free cyanide using flow analysis (FIA and CFA) - Part 2 Method using continuous flow analysis (CFA) (ISO .pdf

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1、October 2012Translation by DIN-Sprachendienst.English price group 13No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS

2、 13.060.50!$|o“1918976www.din.deDDIN EN ISO 14403-2Water quality Determination of total cyanide and free cyanide using flow analysis (FIAand CFA) Part 2: Method using continuous flow analysis (CFA) (ISO 14403-2:2012);English version EN ISO 14403-2:2012,English translation of DIN EN ISO 14403-2:2012-

3、10Wasserbeschaffenheit Bestimmung von Gesamtcyanid und freiem Cyanid mittels Flieanalytik (FIA und CFA) Teil 2: Verfahren mittels kontinuierlicher Durchflussanalyse (CFA) (ISO 14403-2:2012);Englische Fassung EN ISO 14403-2:2012,Englische bersetzung von DIN EN ISO 14403-2:2012-10Qualit de leau Dosage

4、 des cyanures totaux et des cyanures libres par analyse en flux (FIA et CFA) Partie 2: Mthode par analyse en flux continu (CFA) (ISO 14403-2:2012);Version anglaise EN ISO 14403-2:2012,Traduction anglaise de DIN EN ISO 14403-2:2012-10SupersedesDIN EN ISO 14403:2002-07www.beuth.deIn case of doubt, the

5、 German-language original shall be considered authoritative.Document comprises 29 pages09.12 DIN EN ISO 14403-2:2012-10 2 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee ISO/TC 147 “Water quality” in collaboration with Technical Committ

6、ee CEN/TC 230 “Water analysis” (Secretariat: DIN, Germany). The responsible German body involved in its preparation was the Normenausschuss Wasserwesen (Water Practice Standards Committee), Working Group NA 119-01-03-01-05 AK Flieanalysenverfahren of Working Committee NA 119-01-03 AA Wasseruntersuch

7、ung. 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): Part 1: Method using flow injection analysis (FIA) Part 2: Method using continuous flow analysis (CFA) This standard is part of the

8、 series Deutsche Einheitsverfahren zur Wasser-, Abwasser- und Schlammunter-suchung Anionen (Gruppe D) (German standard methods for the examination of water, waste water and sludge Anions (group D) and describes method D 3. Designation of method D 2 “Determination of total cyanide and free cyanide us

9、ing flow analysis (FIA and CFA) Part 2: Method using continuous flow analysis (CFA) (D 3)”: Method DIN EN ISO 14403-2 D 3 Amendments This standard differs from DIN EN ISO 14403:2002-07 as follows: a) the standard has been divided into two parts, the CFA method as specified in ISO 14403:2002-07 is no

10、w dealt with in this standard DIN EN ISO 14403-2 and DIN EN ISO 14403-1 covers the new FIA method; b) the text of the standard has been adjusted accordingly; c) the title of the standard has been adjusted accordingly. Previous editions DIN EN ISO 14403: 2002-07 The DIN Standards corresponding to the

11、 International Standards referred to in this document are as follows: ISO 3696 DIN ISO 3696 ISO 5667-3 DIN EN ISO 5667-3 ISO 5725-2 DIN ISO 5725-2 ISO 8466-1 DIN 38402-51 ISO 8466-2 DIN ISO 8466-2 DIN EN ISO 14403-2:2012-10 3 Expert assistance and specialized laboratories will be required to perform

12、 the analysis described in this standard. Existing safety regulations are to be taken into account. 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. German standard methods for

13、the examination of water, waste water and sludge Standard methods published as DIN Standards are obtainable from Beuth Verlag GmbH, either individually or grouped in volumes. The standard methods included in the loose-leaf publication entitled Deutsche Einheits-verfahren zur Wasser-, Abwasser- und S

14、chlammuntersuchung will continue to be published jointly by Wiley-VCH Verlag GmbH a power of 8 W to 12 W; a digestion coil of borosilicate glass Tuart glass or poltetrauorethlene (PTFE).Suitable dimensions among others (using a 89 lamp emitting at 351 nm) for a digestion coil made of Tuart glass or

15、PTFE are: capacit of approximatel 4 ml (e.g. 30 or 60 turns with a diameter of 30 mm a tube wall thickness of at maximum 1 mm and an internal diameter of 1 mm or 2 mm).For an emission maximum of 312 nm r 5 nm and a digestion coil made of borosilicate glass or Tuart glass or PTFE suitable dimensions

16、among others are: a capacit of approximatel 13 ml (e.g. 45 turns with a diameter of 30 mm).The main criteria for a good choice of 89 lamp and digestion sstem is the results of digestion recover rates (9.3.2).0ake sure that no 89 light with a wavelength below 290 nm reaches the sample ow in order to

17、avoid the decomposition of thiocanate to canide.7.1.6 In-line distillation device adMustable to a temperature of 125 C r 1 C with a distillation coil of glass or polmer material length of coil e.g. 80 cm internal diameter e.g. 15 mm.7.1.7 Manifold capable of highl reproducible dosing of gas bubbles

18、sample and reagents and having appropriate transport sstems and connection assemblies of chemicall inert glass polmer or metal.7.1.8 Heating bath for colorimetric reaction adMustable to a temperature of 37 C r 1 C with a coil volume to allow a sample retention period of approximatel 4 min. 3KRWRPHWU

19、LFGHWHFWRU with a ow cell and having a wavelength range 600 nm r 10 nm.8se an appropriate optical pathlength to achieve a minimum absorbance (absolute value) of 001 per 1 cm pathlength for a 10 g/l canide solution.7.1.10 Recording unit (e.g. strip chart recorder integrator printer and plotter or a c

20、omputer data sstem). In general peak height signals are measured. U is the mass concentration of the standard solutions expressed in micrograms per litre;a is the ordinate intercept expressed in instrument-related units.9.5 Sample measurementAnalse the samples pretreated according to Clause 8 in the

21、 same wa as the calibration solutions with the continuous ow sstem.If the mass concentrations of the samples exceed the validit of the calibrated working range dilute the samples.Check the validit of the calibration function after each sample series but at least after the measurement of 10 to 20 sam

22、ples using one calibration solution each for the lower and upper part of the working range.Recalibrate if necessar.After completion of the measurement the sstem should be rinsed with water (6.1).10 CalculationDetermine the mass concentrations of the samples using the measured values obtained as spec

23、ied in 9.4 for the calibration solutions.Calculate U using ETuation (2): =yab(2)For an explanation of the smbols see 9.4.11 Expression of resultsReport the results to two signicant gures at most.EXAMPLE 1EXAMPLE 2U(total CN)U(free CN)29 102g/l45 g/l12 Test reportThis test report shall contain at lea

24、st the following information:a) the test method used together with a reference to this part of ISO 14403 (ISO 14403-2:2012);b) all information necessar for identication of the sample;c) the tpe of sample pretreatment;d) the canide concentration (free or total canide) in micrograms per litre expresse

25、d in accordance with Clause 11;15DIN EN ISO 14403-2:2012-10 EN ISO 14403-2:2012 (E) e) an special observations noted during the determination;f) an deviations from this part of ISO 14403 which could have affected the result.16DIN EN ISO 14403-2:2012-10 EN ISO 14403-2:2012 (E) Annex A (informative) (

26、DPSOHVRIRZVVWHPVPhotometric CFA congurations other than shown in Figures A.1 and A.2 ma be used provided the meet the criteria of the method and achieve the Tualit control criteria in Clause 9.17DIN EN ISO 14403-2:2012-10 EN ISO 14403-2:2012 (E) KeyR1 buffer p+ 38 for distillation and gas diffusion

27、method (6.21.1)R2 =nSO4solution (6.21.2) for free canide; water (6.1) for total canideR4a buffer solution for nal photometric determination for distillation method (6.21.4.1)R5 chloramine-T solution (6.21.5)R6 colour reagent (6.21.6)1pump (ow rates in millilitres per minute)2 reaction coil: length 5

28、0 cm internal diameter 15 mm3U9 decomposition unit 351 nm4 reaction coil: length 50 cm internal diameter 15 mm5 distillation unit 125 C6 reaction coil: length 50 cm internal diameter 15 m7 reaction coil: length 50 cm internal diameter 15 mm8 heating bath: 37 C length 100 cm internal diameter 2 mm9 d

29、etector (e.g. 1 cm optical pathlength) wavelength 590 nm to 610 nm10 wasteaAir segmentation gas.bSample.cResample.Figure A.1 Example of a CFA system for the spectrometric determination of free and total cyanide JOWRJO ZLWKDGLVWLOODWLRQSURFHGXUH DFFRUGLQJWR 18DIN EN ISO 14403-2:2012-10 EN ISO 14403-2

30、:2012 (E) KeyR1 buffer p+ 38 for distillation and gas diffusion method (6.21.1)R3 recipient solution only for gas diffusion (6.21.3)R4b buffer solution for the nal photometric determination for gas diffusion method (6.21.4.2)R5 chloramine-T solution (6.21.5)R6 colour reagent (6.21.6)1pump (ow rates

31、in millilitres per minute)2 reaction coil: length 50 cm internal diameter 1 mm3U9 decomposition unit: 351 nm 420 cm internal diameter 2 mm4 heating bath: 30 C length 50 cm internal diameter 1 mm5 gas diffusion unit6 reaction coil: length 50 cm internal diameter 1 mm7 reaction coil: length 50 cm inte

32、rnal diameter 1 mm8 heating bath: 37 C length 100 cm internal diameter 1 mm9 detector (e.g. 1 cm optical pathlength) wavelength 590 nm to 610 nm10 wasteaAir segmentation gas.bSample.Figure A.2 Example of a CFA system for the spectrometric determination of free and total cyanide JOWRJO ZLWKJDVGLIIXVL

33、RQVHSDUDWLRQ DFFRUGLQJWR 19DIN EN ISO 14403-2:2012-10 EN ISO 14403-2:2012 (E) Annex B (normative) Determination of the real cyanide concentration in the potassium cyanide solutionB.1 GeneralIf .CN is used to prepare the canide calibration solutions (6.20.5) proceed as follows.B.2 Additional reagents

34、B.2.1 p-Dimethylaminobenzylidene rhodanine.B.2.2 Indicator solution.Dissolve 002 g of p-dimethlaminobenlidene rhodanine (%.2.1) in 100 ml of acetone (C3+6O).This solution is stable for 1 week if stored in a refrigerator at 1 C to 5 C.B.2.3 Silver nitrate solution c(AgNO3) = 1 mmol/l.B.3 Determinatio

35、n of cyanide concentration in potassium cyanide solutionPipette 10 ml of potassium canide solution (6.20.2) into a beaker. Add 025 ml of indicator solution (%.2.2).Titrate with the silver nitrate solution (%.2.3) until the colour changes from ellow to ellow-red (consumption V1).Calculate the canide

36、concentration in the potassium canide solution using ETuation (%.1):CN132CNAgNO=()Vc MV(%.1)whereUCNis the canide contentration in the potassium canide solution (6.20.2) in milligrams per litre;V1is the volume of silver nitrate solution (%.2.3) consumed in millilitres;c(AgNO3) is the concentration o

37、f silver nitrate solution in millimoles per litre;M2CNis the molar mass of 2CN ( = 52 g/mol);V is the volume of the potassium canide solution (6.20.2) in millilitres.20DIN EN ISO 14403-2:2012-10 EN ISO 14403-2:2012 (E) Annex C (informative) Example for the determination of total cyanide and free cya

38、nide by FRQWLQXRXVRZDQDOVLV reference electrode: AgAgCl; auxiliar electrode: platinum; potential applied: 00 9.Other amperometric CFA congurations ma be used provided the meet the criteria of the method and achieve the Tualit control criteria in Clause 9.C.2 Additional bibliography for the applicati

39、on of amperometric detectionSee 7 to 10 and 12.21DIN EN ISO 14403-2:2012-10 EN ISO 14403-2:2012 (E) KeyR1 buffer p+ 38 for distillation and gas diffusion method (6.21.1)R3 recipient solution for gas diffusion (6.21.3)1 pump (ow rates in millilitres per minute)2 reaction coil: length 50 cm internal d

40、iameter 1 mm3U9 decomposition unit: 351 nm length 420 cm internal diameter 2 mm4 heating bath: 30 C length 50 cm internal diameter 1 mm5 gas diffusion unit6 amperometric detector (specication see C.1)7 wasteaAir segmentation gas.bSample.Figure C.1 Example of a CFA system for the amperometric determi

41、nation of free and total cyanide (10 g/l to 100 g/l) gas-diffusion separation (according to C.1)22DIN EN ISO 14403-2:2012-10 EN ISO 14403-2:2012 (E) Annex D (informative) Performance dataAn interlaborator trial for ow analsis sstems as described in Clause 7 was carried out in Spring 2009. The result

42、s are shown in Tables D.1 and D.2.Table D.1 Statistical data for the determination of free cyanide by CFA LQDFFRUGDQFHZLWK,6213)Sample MatrixalnoXxK sRCVRsrCVrg/l g/l g/l g/l 1Drinking water21921130279929221 79045 162Drinking water219300252531011212 84053 213Surface water 21930045436968273 63055 134

43、Surface water 208943303081026232 75045 155 Waste water 18 82 1186050916343 62082 156 Waste water 20 90 3225240961280 117061 25l number of laboratories after outlier reMectionn number of individual test results after outlier reMectiono percentage of outliersX assigned valuexoverall mean of results (w

44、ithout outliers)K recover ratesRreproducibilit standard deviationCVRcoefcient of variation of reproducibilitsrrepeatabilit standard deviationCVrcoefcient of variation of repeatabilitaOrigin of samples:samples 1 2 spiked Cit of %erlinsamples 3 4 spiked Landwehrkanal Cit of %erlinsamples 5 6 spiked Wa

45、ster Water Plant %erlin-Ruhleben23DIN EN ISO 14403-2:2012-10 EN ISO 14403-2:2012 (E) Table D.2 Statistical data for the determination of total cyanide by CFA LQDFFRUGDQFHZLWK,6213)Sample Matrixal noXxK sRCV,RsrCV,rg/l g/l g/l g/l 1Drinking water21939730288961164 57057 202Drinking water20911335047594

46、9232 49078 163Drinking water20919928258923200 77050 194Surface water 188614945452104172 38062 145Surface water 21967755529962265 50105 206Surface water 19816253489923375 77069 147 Waste water 18 84 20060577961300 52068 128 Waste water 19 88 1626359887409 73067 129 Waste water 20 93 11445399887414 104075 1