SIST EN ISO 11206:2013
(Main)Water quality - Determination of dissolved bromate - Method using ion chromatography (IC) and post column reaction (PCR) (ISO 11206:2011)
Water quality - Determination of dissolved bromate - Method using ion chromatography (IC) and post column reaction (PCR) (ISO 11206:2011)
This 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 pretreatment of the sample (e.g. dilution) allows determination of bromate at concentrations 0,5 μg/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.
Wasserbeschaffenheit - Bestimmung von gelöstem Bromat - Verfahren mittels Ionenchromatographie (IC) und Nachsäulenreaktion (PCR) (ISO 11206:2011)
Diese Internationale Norm legt ein Verfahren zur Bestimmung von gelöstem Bromat in Wasser (z. B. Trinkwasser, Mineralwasser, Rohwasser, Oberflächenwasser, teilweise behandeltes Wasser oder Badewasser) fest.
Eine geeignete Probenvorbehandlung (z. B. Verdünnung) erlaubt die Bestimmung von Bromatkonzentrationen ≥ 0,5 µg/l.
Der Arbeitsbereich ist durch die Kapazität der Trennsäule begrenzt. Eine Probenverdünnung in den Arbeitsbereich kann erforderlich sein.
Qualité de l'eau - Détermination du bromate dissous - Méthode utilisant la chromatographie ionique (IC) et la réaction post-colonne (PCR) (ISO 11206:2011)
L'ISO 11206:2011 spécifie une méthode pour le dosage du bromate dissous dans l'eau (par exemple l'eau potable, l'eau minérale, l'eau brute, les eaux de surface, l'eau partiellement traitée ou l'eau de piscine).
Le prétraitement approprié de l'échantillon (par exemple dilution) permet de doser le bromate à des concentrations supérieures ou égales à 0,5 µg/l.
Le domaine de travail est limité à la capacité d'échange ionique de la colonne de séparation. Il peut être nécessaire de diluer l'échantillon dans le domaine de travail du bromate.
Kakovost vode - Določevanje raztopljenega bromata - Metoda z ionsko kromatografijo in pokolonsko reakcijo (PCR) (ISO 11206:2011)
Ta mednarodni standard določa metodo za določevanje raztopljenega bromata v vodi (npr. pitna, mineralna, surova, površinska, delno pripravljena ali bazenska voda). Ustrezna predpriprava vzorca (npr. redčenje) omogoča določevanje bromata pri koncentraciji 0,5 μg/l. Delovni obseg je omejen z zmogljivostjo ionske izmenjave separatorske kolone. Morda je potrebno redčenje vzorca do delovnega obsega bromata.
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 11206:2013
01-julij-2013
.DNRYRVWYRGH'RORþHYDQMHUD]WRSOMHQHJDEURPDWD0HWRGD]LRQVNR
NURPDWRJUDILMRLQSRNRORQVNRUHDNFLMR 3&5 ,62
Water quality - Determination of dissolved bromate - Method using ion chromatography
(IC) and post column reaction (PCR) (ISO 11206:2011)
Wasserbeschaffenheit - Bestimmung von gelöstem Bromat - Verfahren mittels
Ionenchromatographie (IC) und Nachsäulenreaktion (PCR) (ISO 11206:2011)
Qualité de l'eau - Détermination du bromate dissous - Méthode utilisant la
chromatographie ionique (IC) et la réaction post-colonne (PCR) (ISO 11206:2011)
Ta slovenski standard je istoveten z: EN ISO 11206:2013
ICS:
13.060.50 3UHLVNDYDYRGHQDNHPLþQH Examination of water for
VQRYL chemical substances
SIST EN ISO 11206:2013 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
SIST EN ISO 11206:2013
---------------------- Page: 2 ----------------------
SIST EN ISO 11206:2013
EUROPEAN STANDARD
EN ISO 11206
NORME EUROPÉENNE
EUROPÄISCHE NORM
March 2013
ICS 13.060.50
English Version
Water quality - Determination of dissolved bromate - Method
using ion chromatography (IC) and post column reaction (PCR)
(ISO 11206:2011)
Qualité de l'eau - Détermination du bromate dissous - Wasserbeschaffenheit - Bestimmung von gelöstem Bromat
Méthode utilisant la chromatographie ionique (IC) et la - Verfahren mittels Ionenchromatographie (IC) und
réaction post-colonne (PCR) (ISO 11206:2011) Nachsäulenreaktion (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 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 version 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, 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, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United
Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2013 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 11206:2013: E
worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST EN ISO 11206:2013
EN ISO 11206:2013 (E)
Contents Page
Foreword . 3
2
---------------------- Page: 4 ----------------------
SIST EN ISO 11206:2013
EN ISO 11206:2013 (E)
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 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 September 2013, and conflicting national standards shall be
withdrawn at the latest by September 2013.
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] 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, 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,
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.
3
---------------------- Page: 5 ----------------------
SIST EN ISO 11206:2013
---------------------- Page: 6 ----------------------
SIST EN ISO 11206:2013
INTERNATIONAL ISO
STANDARD 11206
First edition
2011-07-01
Water quality — Determination of
dissolved bromate — Method using ion
chromatography (IC) and post column
reaction (PCR)
Qualité de l’eau — Détermination du bromate dissous — Méthode utilisant
la chromatographie ionique (IC) et la réaction post-colonne (PCR)
Reference number
ISO 11206:2011(E)
©
ISO 2011
---------------------- Page: 7 ----------------------
SIST EN ISO 11206:2013
ISO 11206:2011(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2011
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,
electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISO’s
member body in the country of the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2011 – All rights reserved
---------------------- Page: 8 ----------------------
SIST EN ISO 11206:2013
ISO 11206:2011(E)
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Interferences . 1
4 Principle . 1
5 Reagents . 2
6 Apparatus . 4
7 Quality requirements . 5
7.1 Separator column . 5
7.2 PCR conditions . 6
7.3 Chromatographic and PCR conditions for the chromatogram shown in Figure 3 . 7
7.4 Chromatographic and PCR conditions for the chromatogram shown in Figure 4 . 8
8 Sampling and sample pretreatment . 9
9 Procedure .10
9.1 General .10
9.2 Calibration .10
9.3 Measurement of bromate .10
9.4 Chlorite removal .10
9.5 Validity check of the calibration function . 11
10 Calculation . 11
11 Expression of results . 11
12 Test report . 11
Annex A (informative) Precision data .12
Bibliography .15
© ISO 2011 – All rights reserved iii
---------------------- Page: 9 ----------------------
SIST EN ISO 11206:2013
ISO 11206:2011(E)
Foreword
ISO (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 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 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 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 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 11206 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical,
chemical and biochemical methods.
iv © ISO 2011 – All rights reserved
---------------------- Page: 10 ----------------------
SIST EN ISO 11206:2013
INTERNATIONAL 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 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.
IMPORTANT — It is absolutely essential that tests conducted according to this International Standard
be carried out by suitably trained staff.
1 Scope
This 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 pretreatment of the sample (e.g. dilution) allows determination of bromate at concentrations �0,5 µg/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 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 3696, Water for analytical laboratory use — Specification and test methods
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
ISO 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 functions
3 Interferences
Metals 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 exchangers (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 accordance 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 analyte’s retention time. Sample
dilution and/or gradient elution overcomes much interference.
4 Principle
The 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 acids (e.g. sulfuric acid) or aqueous solutions of salts of weak monobasic acids
© ISO 2011 – All rights reserved 1
---------------------- Page: 11 ----------------------
SIST EN ISO 11206:2013
ISO 11206:2011(E)
and 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 electrochemically prepared) (5.13).
−
Detection of bromate [�(BrO ) � 0,5 µg/l] is achieved by applying an acidic solution of potassium iodide
3
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 measured by its UV absorption at 352 nm.
[2] [3] [4]
NOTE This method can be combined with ISO 10304-1 , ISO 10304-4 , and ISO 15061 .
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 validity 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 Reagents
Use only reagents of pro analysis grade. Weigh the reagents with an accuracy of �1 % of the nominal mass,
unless 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, Na CO .
2 3
5.3 Sulfuric acid, �(HSO ) � 1 mol/l.
2 4
5.4 Sodium hydroxide, NaOH.
5.5 Potassium hydroxide, KOH.
5.6 Sodium hydrogencarbonate, NaHCO .
3
5.7 Ammonium heptamolybdate tetrahydrate, (NH ) Mo O �4HO.
4 6 7 24 2
5.8 Potassium iodide, KI.
5.9 Nitric acid, �(HNO ) � 1,41 g/ml.
3
5.10 Iron(II) sulfate heptahydrate, FeSO�7HO.
4 2
5.11 Potassium bromate, KBrO .
3
5.12 Ethylenediamine, C H N , 99 %.
2 8 2
5.13 Eluents.
Degas all eluents used. Take steps to 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 specified 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.
2 © ISO 2011 – All rights reserved
---------------------- Page: 12 ----------------------
SIST EN ISO 11206:2013
ISO 11206:2011(E)
5.13.1 Sodium carbonate concentrate, �(NaCO ) � 0,09 mol/l.
2 3
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 stable for 6 months if stored at 2 °C to 8 °C.
5.13.2 Sodium carbonate eluent, �(NaCO ) � 0,009 mol/l.
2 3
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).
5.13.3 Sulfuric acid eluent, �(HSO ) � 0,1 mol/l.
2 4
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 the PCR reagent in the PCR unit (5.15).
5.14 Ammonium heptamolybdate solution, �[(NH) Mo O ] � 0,002 mol/l.
4 6 7 24
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 Post 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
heptamolybdate 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 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 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.
2+
5.16 Iron(II) solution, �(Fe ) � 1 000 mg/l.
Place 6 µl of nitric acid (5.9) in approximately 15 ml water (5.1) in a 25 ml volumetric 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, �(BrO ) � 1 000 mg/l.
3
Dry approximately 1,5 g of potassium bromate (5.11) for at least 1 h at 105 °C � 5 °C. Store the dried solid in
a desiccator.
© ISO 2011 – All rights reserved 3
---------------------- Page: 13 ----------------------
SIST EN ISO 11206:2013
ISO 11206:2011(E)
Dissolve 1,306 g � 0,001 g of the dried potassium bromate in approximately 800 ml of water (5.1) in a 1 000 ml
volumetric flask and dilute to volume with water (5.1). Store the solution at 2 °C to 8 °C in polyethene or glass
bottles and renew it every 12 months.
Alternatively, use commercially available stock solutions of the required concentration.
5.18 Bromate standard solution.
Depending on the concentrations expected, prepare the following standard solutions of different bromate
concentrations from the stock stand
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.