DIN EN ISO 23913-2009 Water quality - Determination of chromium(VI) - Method using flow analysis (FIA and CFA) and spectrometric detection (ISO 23913 2006) English version of DIN E.pdf

1、September 2009DEUTSCHE NORM English price group 12No part of this standard 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 13.060.50!$YVh“15451

2、69www.din.deDDIN EN ISO 23913Water quality Determination of chromium(VI) Method using flow analysis (FIA and CFA) and spectrometric detection(ISO 23913:2006)English version of DIN EN ISO 23913:2009-09Wasserbeschaffenheit Bestimmung von Chrom(VI) Verfahren mittels Flieanalytik (FIA und CFA) und spekt

3、rometrischer Detektion(ISO 23913:2006)Englische Fassung DIN EN ISO 23913:2009-09www.beuth.deDocument comprises 22 pagesDIN EN ISO 23913:2009-09 2 National foreword This standard has been prepared by Technical Committee ISO/TC 147 “Water quality” in collaboration with Technical Committee CEN/TC 230 “

4、Water analysis” (Secretariat: DIN, Germany). The responsible German body involved in its preparation was the Normenausschuss Wasserwesen (Water Practice Standards Committee), Technical Committees NA 119-01-03-01-05 AK Flieanalyseverfahren and NA 119-01-03 AA Wasseruntersuchung. This standard is part

5、 of the series Deutsche Einheitsverfahren zur Wasser-, Abwasser- und Schlamm-untersuchung Anionen (Gruppe D) (German standard methods for the examination of water, waste water and sludge Anions (group D) and describes method D 41. Designation of method D 41 “Determination of chromium(VI) Method usin

6、g flow analysis (FIA and CFA) and spectrometric detection”: Method DIN EN ISO 23913 D 41 English version of DIN EN ISO 23913:2009-09. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 3696 DIN ISO 3696 ISO 5667-3 DIN EN ISO 5667-3 ISO 846

7、6-1 DIN 38402-51 Expert assistance and specialized laboratories will be required to perform 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 t

8、o what extent additional conditions will have to be specified. German standard methods for 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 t

9、he loose-leaf publication entitled Deutsche Einheits-verfahren zur Wasser-, Abwasser- und Schlammuntersuchung will continue to be published jointly by Wiley-VCH Verlag and Beuth Verlag GmbH. All standard methods relevant to the Abwasserverordnung (Waste Water Regulation) (AbwV1) included in the new

10、Regulation on Section 7a of the Gesetz zur Ordnung des Wasserhaushaltes (German Water Management Act1) concerning Anforderungen an das Einleiten von Abwasser in Gewsser together with the Abwasserverordnung and the Gesetz zur Ordnung des Wasserhaushalts have been published by Beuth-Verlag GmbH as a l

11、oose-leaf collection Analysenverfahren in der Abwasserverordnung Rechtsvorschriften und Normen (Supplements). Standards or draft standards bearing the group title “German standard methods for the examination of water, waste water and sludge” are classified under the following categories (main titles

12、): 1)Registered in the DITR database of DIN Software GmbH, obtainable from: Beuth Verlag GmbH, 10772 Berlin. As a result of national implementation in Germany, the following action has been taken: The units and sample numbers missing in Table B.2 of ISO 23913 have been completed in the German and DI

13、N EN ISO 23913:2009-09 3 General information (group A) (DIN 38402) Sensory analysis (group B) (DIN 38403) Physical and physicochemical parameters (group C) (DIN 38404) Anions (group D) (DIN 38405) Cations (group E) (DIN 38406) Substance group analysis (group F) (DIN 38407) Gaseous constituents (grou

14、p G) (DIN 38408) Parameters characterizing effects and substances (group H) (DIN 38409) Biological-ecological methods of analysis (group M) (DIN 38410) Microbiological methods (group K) (DIN 38411) Test methods using water organisms (group L) (DIN 38412) Individual constituents (group P) (DIN 38413)

15、 Sludge and sediments (group S) (DIN 38414) Bio-assays with microorganisms (group T) (DIN 38415) In addition to the methods described in the DIN 38402 to DIN 38415 series of standards, there are a number of European and International Standards available as DIN EN, DIN EN ISO and DIN ISO Standards, w

16、hich also form part of the collection of German standard methods. Information on Parts of these series of standards that have already been published can be obtained from the offices of the Normenausschuss Wasserwesen, telephone +49 30 2601-2448, or from Beuth Verlag GmbH, Burggrafenstr. 6, 10787 Ber

17、lin. National Annex NA (informative) Bibliography DIN 38402-51, German standard methods for the examination of water, waste water and sludge General information (group A) Calibration of analytical methods, evaluation of analytical results and linear calibration functions used to determine the perfor

18、mance characteristics of analytical methods (A 51) DIN ISO 3696, Water for analytical laboratory use Specification and test methods DIN EN ISO 5667-3, Water quality Sampling Part 3: Guidance on the preservation and handling of water samples DIN EN ISO 23913:2009-09 4 This page is intentionally blank

19、 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 23913 May 2009 ICS 13.060.50 English Version Water quality - Determination of chromium(VI) - Method using flow analysis (FIA and CFA) and spectrometric detection (ISO 23913:2006) Qualit de leau - Dosage du chrome(VI) - Mthode par analyse en f

20、lux (FIA et CFA) et dtection spectromtrique (ISO 23913:2006) Wasserbeschaffenheit - Bestimmung von Chrom(VI) - Verfahren mittels Flieanalytik (FIA und CFA) und spektrometrischer Detektion (ISO 23913:2006) This European Standard was approved by CEN on 14 May 2009. CEN members are bound to comply with

21、 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-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN Management Cen

22、tre 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 responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as the offici

23、al versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slove

24、nia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2009 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN na

25、tional Members. Ref. No. EN ISO 23913:2009: EContents Page Foreword .3 Introduction.4 1 Scope5 2 Normative references5 3 Principle .5 4 Interferences 6 5 Reagents 6 6 Apparatus.9 7 Sampling and sample preparation.10 8 Procedure.10 9 Determination 11 10 Expression of results12 11 Test report12 Annex

26、A (informative) Examples of flow analysis systems for the determination of chromium(VI)13 Annex B (informative) Performance characteristics .16 Bibliography18 2 EN ISO 23913:2009 (E) DIN EN ISO 23913:2009-09 Foreword 3 The text of ISO 23913:2006 has been prepared by Technical Committee ISO/TC 147 “W

27、ater quality” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 23913:2009 by 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 public

28、ation of an identical text or by endorsement, at the latest by November 2009, and conflicting national standards shall be withdrawn at the latest by November 2009. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC

29、 shall not be held responsible for identifying any or all such patent rights. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark,

30、 Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 23913:2006 has been approved b

31、y CEN as EN ISO 23913:2009 without any modification. EN ISO 23913:2009 (E) DIN EN ISO 23913:2009-09 Introduction Methods using flow analysis automatic wet chemical procedures are particularly suitable for the processing of many analytes in water, in large sample series at a high analysis frequency.

32、Analysis can be performed by flow injection analysis (FIA)1, 2and continuous flow analysis (CFA). 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 s

33、ample preparation may be integrated in the manifold. The reaction product is measured in a flow detector (e.g. flow photometer). It should be investigated whether and to what extent particular problems will require the specification of additional marginal conditions. 4 EN ISO 23913:2009 (E) DIN EN I

34、SO 23913:2009-09 WARNING Persons using this International Standard should be familiar with normal laboratory practice. This standard 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 healt

35、h practices and to ensure compliance with any national regulatory conditions. IMPORTANT It is absolutely essential that tests conducted according to this International Standard are carried out by suitably qualified staff. 1 Scope This International Standard specifies flow injection analysis (FIA) an

36、d continuous flow analysis (CFA) methods for the determination of chromium(VI) in various types of water. The method applies to the following mass concentration ranges. FIA: 20 g/l to 200 g/l and 200 g/l to 2 000 g/l for surface water, leachates and waste water. CFA: 2 g/l to 20 g/l and 20 g/l to 20

37、0 g/l for drinking water, ground water, surface water, leachates and waste water. The range of application may be changed by varying the operating conditions. Seawater may be analysed by these methods with changes in sensitivity and after adaptation of the reagent and calibration solutions to the sa

38、linity 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 applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO

39、 3696, Water for analytical laboratory use Specification and test methods 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 performance characteristics Par

40、t 1: Statistical evaluation of the linear calibration function 3 Principle Chromium(VI) reacts with 1,5-diphenylcarbazide (DPC) to form a red-violet chromium-1,5-diphenylcarbazone complex. The absorbance of this complex is measured at 544 nm 10 nm (maximum absorbance at 544 nm). 5 EN ISO 23913:2009

41、(E) DIN EN ISO 23913:2009-09 4 Interferences Reducing agents in the sample may lead to negative bias for the chromium(VI) concentration. Nitrite does not interfere with the method under the reaction conditions. Concentrations of sulfide exceeding 0,2 mg/l interfere with the method. Oxidizing agents

42、for disinfection in drinking water production like chlorine, chlorine dioxide, ozone and hydrogen peroxide do not interfere with the method provided their mass concentration does not exceed the concentrations given in Table 1. Table 1 Mass concentrations of single disinfection agents not producing s

43、ignificant interference under the given measuring conditions Concentration Disinfectant mg/l Chlorine 0,6 Chlorine dioxide 0,4 Hydrogen peroxide 0,2 Ozone 0,1 Other oxidizing agents like peroxoacetic acid, or permanganate may interfere in the chromium(VI) determination. This shall be considered in t

44、he results. Strongly alkaline or buffered samples may cause negative bias. This effect may be tested by adding 1 part of acid mixture (5.5.1 or 5.5.2) to 3 parts of the sample. This mixture shall have a pH of 1. Otherwise, pretreat the samples with acids (HCl, H2SO4) until the above mentioned test l

45、eads to sufficient results. Iron (III) ions exceeding 10 mg/l interfere with the methods. In the range of 10 mg/l to 100 mg/l, iron (III) ions may lead to a negative bias of up to 8 %. Coloured or turbid samples can cause a bias. To avoid bias, measure the sample again using solution 5.17 instead of

46、 solution 5.10 for feeding line “R2” in Figures A.1 to A.3. Subtract the result of this measurement ysfrom the term y in Equation (2). 5 Reagents Use analytical grade chemicals unless otherwise specified. 5.1 Water, complying to grade 1 as defined in ISO 3696. The chromium blank value shall be check

47、ed (see 8.3). 5.2 Sulfuric acid, (H2SO4 ) = 1,84 g/ml. 5.3 Orthophosphoric acid, (H3PO4) = 1,71 g/ml. 5.4 Surfactant solution, aqueous polyethylene glycol dodecyl ether, HO-(CH2-CH2O)nC12H21, with a mass fraction of 30 %. 6 EN ISO 23913:2009 (E) DIN EN ISO 23913:2009-09 5.5 Acid mixtures. 5.5.1 Acid

48、 mixture for FIA, (R1 in Figure A.1). Add to a 250 ml volumetric flask about 125 ml of water (5.1). Add 29 ml of sulfuric acid (5.2) and 31 ml of orthophosphoric acid (5.3), mix and bring to volume with water (5.1). This solution acidifies the reaction mixture passing the detector to a necessary pH

49、of 1. The solution is stable for up to 1 year if stored at room temperature. 5.5.2 Acid mixture for CFA, (R1 in Figures A.2 and A.3). Add 1 ml of surfactant solution (5.4) to 200 ml of acid mixture for FIA (5.5.1). The solution is stable for up to 1 week if stored at room temperature. 5.6 1,5-diphenylcarbazide, C13H14N4O. 5.7 Acetone, C3H6O. 5.8 1-Propanol, C3H8O. 5.9 Potassium dichromate, K2Cr2O7. 5.10 Diphenylcarbazide solution, (R2 in Figures A.1 to A.3). Dissolve in a 250 ml beaker 0,43 g of 1,5-di