1、BSI Standards PublicationBS EN ISO 11206:2013Water quality Determinationof dissolved bromate Method using ionchromatography (IC) and postcolumn reaction (PCR)BS EN ISO 11206:2013 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO 11206:2013. It is identical to
2、ISO 11206:2011.The UK participation in its preparation was entrusted to Technical Committee EH/3, Water quality.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. U
3、sers are responsible for its correct application. The British Standards Institution 2013.Published by BSI Standards Limited 2013ISBN 978 0 580 79501 5ICS 13.060.50Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority
4、of the Standards Policy and Strategy Committee on 30 November 2013.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 11206 March 2013 ICS 13.060.50 English Version Water quality - Determination of dissolved bromate - Me
5、thod using ion chromatography (IC) and post column reaction (PCR) (ISO 11206:2011) Qualit de leau - Dosage du bromate dissous - Mthode utilisant la chromatographie ionique (IC) et la raction post-colonne (PCR) (ISO 11206:2011) Wasserbeschaffenheit - Bestimmung von gelstem Bromat - Verfahren mittels
6、Ionenchromatographie (IC) und Nachsulenreaktion (PCR) (ISO 11206:2011) This European Standard was approved by CEN on 10 February 2013. 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 national s
7、tandard 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 version i
8、n 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, Czech
9、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. EURO
10、PEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2013 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 11206:2013: EBS EN ISO 1
11、1206:2013EN ISO 11206:2013 (E) 3 Foreword The text of ISO 11206:2011 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 11206:2013 by Technical Committee CEN/TC 230 “Water analysis” the sec
12、retariat 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 September 2013, and conflicting national standards shall be withdrawn at the latest by September 2013. Attention i
13、s drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC 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 fo
14、llowing countries are bound 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
15、, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 11206:2011 has been approved by CEN as EN ISO 11206:2013 without any modification. BS EN ISO 11206:2013ISO 11206:2011(E)Contents PageForeword iv1 Sco
16、pe 12 Normative references .13 Interferences .14 Principle .15 Reagents 26 Apparatus 47 Quality requirements 57.1 Separator column 57.2 PCR conditions 67.3 Chromatographic and PCR conditions for the chromatogram shown in Figure 3 77.4 Chromatographic and PCR conditions for the chromatogram shown in
17、Figure 4 88 Sampling and sample pretreatment .99 Procedure 109.1 General .109.2 Calibration .109.3 Measurement of bromate 109.4 Chlorite removal 109.5 Validity check of the calibration function .1110 Calculation 1111 Expression of results .1112 Test report .11Annex A (informative) Precision data 12B
18、ibliography .15 ISO 2011 All rights reserved iiiBS EN ISO 11206:2013ForewordISO (the International Organization 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
19、 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 liaison with ISO, also take part in the work. ISO collaborates closely with
20、 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 technical committees is to prepare International Standards. Draft Internat
21、ional 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 drawn to the possibility that some of the elements of this document may be
22、the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights.ISO 11206 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical, chemical and biochemical methods.ISO 11206:2011(E)iv ISO 2011 All rights reservedBS EN I
23、SO 11206:2013INTERNATIONAL STANDARD ISO 11206:2011(E)Water quality Determination of dissolved bromate Method using ion chromatography (IC) and post column reaction (PCR)WARNING Persons using this International Standard should be familiar with normal laboratory practice. This standard does not purpor
24、t 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.IMPORTANT It is absolutely essential that tests conducted according to
25、this International Standard be carried out by suitably trained staff.1 ScopeThis International Standard specifies a method for the determination of dissolved bromate in water (e.g. drinking water, mineral water, raw water, surface water, partially treated water or swimming pool water).Appropriate pr
26、etreatment of the sample (e.g. dilution) allows determination of bromate at concentrations null0,5 g/l.The working range is restricted by the ion-exchange capacity of the separator column. Dilution of the sample to the bromate working range can be necessary.2 Normative referencesThe following refere
27、nced 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 analytical laboratory use Specification and test m
28、ethodsISO 8466-1, Water quality Calibration and evaluation of analytical methods and estimation of performance characteristics Part 1: Statistical evaluation of the linear calibration functionISO 8466-2, Water quality Calibration and evaluation of analytical methods and estimation of performance cha
29、racteristics Part 2: Calibration strategy for non-linear second order calibration functions3 InterferencesMetals present in samples and eluents bind to the resin material of the separator column, resulting in a loss of performance. Metal ions can be eliminated with the aid of special cation exchange
30、rs (see 6.2 and Clause 8, Note 1).Solid particles and organic compounds (e.g. mineral oils, detergents, and humic acids) shorten the lifetime of the precolumn and the separator column (see Clause 8, Notes 2 and 3).Chlorite can interfere with the determination of bromate. Remove chlorite in accordanc
31、e with the procedure specified in 9.4, if necessary.NOTE Any substance that has a retention time coinciding with bromate and that produces a detector response can interfere. A high concentration of ions can have an impact on the resolution and on the analytes retention time. Sample dilution and/or g
32、radient elution overcomes much interference.4 PrincipleThe sample is pretreated in order to remove ozone, chlorine dioxide, chlorite, metals and solids, if necessary (see Clause 8). Bromate is separated by ion chromatography (IC). An anion exchange resin is used as the stationary phase and either ac
33、ids (e.g. sulfuric acid) or aqueous solutions of salts of weak monobasic acids ISO 2011 All rights reserved 1BS EN ISO 11206:2013and dibasic acids are used as eluents for isocratic or gradient elution (e.g. carbonate-, hydrogen carbonate-, hydroxide-eluent, e.g. manually, automatically or in situ el
34、ectrochemically prepared) (5.13).Detection of bromate null(BrO3) null 0,5 g/l is achieved by applying an acidic solution of potassium iodide containing a catalytic amount of molybdenum(VI), where the bromate reacts with iodide to form the tri-iodide ion in a post column reaction (PCR) step, which is
35、 measured by its UV absorption at 352 nm.NOTE This method can be combined with ISO 10304-12, ISO 10304-43, and ISO 150614.The concentration of bromate is determined after a calibration according to ISO 8466-1 or ISO 8466-2 of the overall procedure.Control experiments are necessary to check the valid
36、ity of the calibration function (9.5). Replicate determinations can be necessary. Use of the method of standard addition may be required if matrix interferences are expected (9.3).5 ReagentsUse only reagents of pro analysis grade. Weigh the reagents with an accuracy of null1 % of the nominal mass, u
37、nless stated otherwise. Prepare alternative volumes of solutions as described in 5.13 to 5.19, if necessary.5.1 Water, ISO 3696, grade 1.5.2 Sodium carbonate, Na2CO3.5.3 Sulfuric acid, null(H2SO4) null 1 mol/l.5.4 Sodium hydroxide, NaOH.5.5 Potassium hydroxide, KOH.5.6 Sodium hydrogencarbonate, NaHC
38、O3.5.7 Ammonium heptamolybdate tetrahydrate, (NH4)6Mo7O24null4H2O.5.8 Potassium iodide, KI.5.9 Nitric acid, null(HNO3) null 1,41 g/ml.5.10 Iron(II) sulfate heptahydrate, FeSO4null7H2O.5.11 Potassium bromate, KBrO3.5.12 Ethylenediamine, C2H8N2, 99 %.5.13 Eluents.Degas all eluents used. Take steps to
39、avoid any renewed air pick-up during operation (e.g. by helium sparging, in-line degasser).The choice of eluent depends on the choice of column and detector; seek advice from the column supplier. The chosen combination of separator column and eluent shall conform to the resolution requirements speci
40、fied in Clause 7. Use eluents as long as the requirements in Clause 7 and in 9.3 are met.A selection of reagents for common eluents is presented in 5.2 to 5.6. Examples for appropriate eluents are given in 5.13.2 and 5.13.3.ISO 11206:2011(E)2 ISO 2011 All rights reservedBS EN ISO 11206:20135.13.1 So
41、dium carbonate concentrate, null(Na2CO3) null 0,09 mol/l.The addition of the following eluent concentrate is appropriate for the eluent preparation (5.13.2):Dissolve 9,54 g of sodium carbonate (5.2) in water (5.1) in a 1 000 ml volumetric flask and dilute to volume with water (5.1).The solution is s
42、table for 6 months if stored at 2 C to 8 C.5.13.2 Sodium carbonate eluent, null(Na2CO3) null 0,009 mol/l.The following eluent is applicable for the determination of bromate:Place 100 ml of the sodium carbonate concentrate (5.13.1) in a 1 000 ml volumetric flask and dilute to volume with water (5.1).
43、5.13.3 Sulfuric acid eluent, null(H2SO4) null 0,1 mol/l.Place 100 ml of sulfuric acid (5.3) in a 1 000 ml volumetric flask and dilute to volume with water (5.1).NOTE Ammonium heptamolybdate tetrahydrate (5.7) can be added to the eluent provided the composition meets the resulting concentration of th
44、e PCR reagent in the PCR unit (5.15).5.14 Ammonium heptamolybdate solution, null(NH4)6Mo7O24 null 0,002 mol/l.Dissolve 0,25 g of ammonium heptamolybdate tetrahydrate (5.7) in 100 ml of water (5.1).The solution is stable for 1 month if stored in a light impervious bottle at ambient temperature.5.15 P
45、ost column reaction (PCR) reagent.Degas all water used for the preparation of the PCR reagent. Take steps to avoid any renewed air pick-up during operation (e.g. by helium sparging).Dissolve 45 g of potassium iodide (5.8) in approximately 500 ml of water (5.1), add 25 ml of the ammonium heptamolybda
46、te solution (5.14) in a 1 000 ml volumetric flask and dilute to volume with water (5.1).Sparge the solution with helium for 20 min to remove all traces of dissolved oxygen, and immediately place it in the PCR module and pressurize it with helium.The solution contains 0,27 mol/l potassium iodide and
47、0,05 mmol/l of ammonium heptamolybdate. Prepare the solution on the day of use. Store the solution in light-impervious bottles (e.g. wrapped with aluminium foil) and protect the solution from light exposure.NOTE Since potassium iodide is photosensitive, the solution can develop a light yellow colour
48、 with time, even when stored under helium. This can be avoided by the addition of sodium hydroxide (5.4) with a resulting concentration of 0,001 mol/l of sodium hydroxide.5.16 Iron(II) solution, null(Fe2+) null 1 000 mg/l.Place 6 l of nitric acid (5.9) in approximately 15 ml water (5.1) in a 25 ml v
49、olumetric flask, dissolve 0,124 g of iron(II) sulfate heptahydrate (5.10) and dilute to volume with water (5.1).The resulting pH value is about 2. The solution is stable for 2 d.5.17 Bromate stock standard solution, null(BrO3) null 1 000 mg/l.Dry approximately 1,5 g of potassium bromate (5.11) for at least 1 h at 105 C null 5 C. Store the dried solid in a desiccator.ISO 11206:2011(E) ISO 2011 All rights reserved 3BS EN ISO 11206:2013Dissolve 1,306 g null 0,001 g of the dried potassium bromate in approximately 800 ml of
