Water quality - Determination of chromium(VI) - Method using flow analysis (FIA and CFA) and spectrometric detection (ISO 23913:2006)

ISO 23913:2006 specifies flow injection analysis (FIA) and 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: for FIA (20 to 200 micrograms per litre and 200 to 2 000 micrograms per litre for surface water, leachates and waste water) and for CFA (2 to 20 micrograms per litre and 20 to 200 micrograms per litre 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 salinity of the samples.

Wasserbeschaffenheit - Bestimmung von Chrom(VI) - Verfahren mittels Fließanalytik (FIA und CFA) und spektrometrischer Detektion (ISO 23913:2006)

Diese Internationale Norm legt ein FIA  und ein CFA Verfahren für die Bestimmung von Chrom(VI) in verschiedenen Wasserarten fest. Das Verfahren ist anwendbar für folgende Konzentrationsbereiche:
   FIA: 20 µg/l bis 200 µg/l und 200 µg/l bis 2 000 µg/l für Oberflächenwasser, Sickerwasser und Abwasser;
   CFA: 2 µg/l bis 20 µg/l und 20 µg/l bis 200 µg/l für Trinkwasser, Grundwasser, Oberflächenwasser, Sickerwasser und Abwasser.
Der Anwendungsbereich kann durch Variation der Versuchsbedingungen geändert werden.
Meerwasser kann mit diesem Verfahren unter Änderungen in der Empfindlichkeit analysiert werden, wenn die Reagenzien und die Bezugslösungen an die Salinität der Proben angepasst werden.

Qualité de l'eau - Dosage du chrome(VI) - Méthode par analyse en flux (FIA et CFA) et détection spectrométrique (ISO 23913:2006)

L'ISO 23913:2006 spécifie deux méthodes: l'analyse avec injection en flux (FIA) et l'analyse en flux continu (CFA) pour le dosage du chrome(VI) dans divers types d'eau. Ces méthodes s'appliquent aux domaines de concentration massique suivants: pour la FIA (20 à 200 microgrammes par litre et 200 à 2 000 microgrammes par litre pour les eaux de surface, les lixiviats et les eaux résiduaires) et pour la CFA (2 à 20 microgrammes par litre et 20 à 200 microgrammes par litre pour l'eau potable, les eaux de surface, les lixiviats et les eaux résiduaires). Le domaine d'application peut varier en fonction des conditions d'utilisation. L'eau de mer peut être analysée par ces méthodes si l'on change la sensibilité et si l'on adapte les solutions de réactifs et d'étalonnage à la salinité des échantillons.

Kakovost vode - Določevanje kroma (VI) - Metoda s pretočno analizo (FIA in CFA) in spektrometrijsko detekcijo (ISO 23913:2006)

General Information

Status
Published
Publication Date
26-May-2009
Technical Committee
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Due Date
27-May-2009
Completion Date
27-May-2009

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SLOVENSKI STANDARD
SIST EN ISO 23913:2009
01-december-2009
.DNRYRVWYRGH'RORþHYDQMHNURPD 9, 0HWRGDVSUHWRþQRDQDOL]R ),$LQ&)$
LQVSHNWURPHWULMVNRGHWHNFLMR ,62

Water quality - Determination of chromium(VI) - Method using flow analysis (FIA and

CFA) and spectrometric detection (ISO 23913:2006)

Wasserbeschaffenheit - Bestimmung von Chrom(VI) - Verfahren mittels Fließanalytik

(FIA und CFA) und spektrometrischer Detektion (ISO 23913:2006)

Qualité de l'eau - Dosage du chrome(VI) - Méthode par analyse en flux (FIA et CFA) et

détection spectrométrique (ISO 23913:2006)
Ta slovenski standard je istoveten z: EN ISO 23913:2009
ICS:
13.060.50 3UHLVNDYDYRGHQDNHPLþQH Examination of water for
VQRYL chemical substances
SIST EN ISO 23913:2009 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 23913:2009
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SIST EN ISO 23913:2009
EUROPEAN STANDARD
EN ISO 23913
NORME EUROPÉENNE
EUROPÄISCHE NORM
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)

Qualité de l'eau - Dosage du chrome(VI) - Méthode par Wasserbeschaffenheit - Bestimmung von Chrom(VI) -

analyse en flux (FIA et CFA) et détection spectrométrique Verfahren mittels Fließanalytik (FIA und CFA) und

(ISO 23913:2006) spektrometrischer Detektion (ISO 23913:2006)
This European Standard was approved by CEN on 14 May 2009.

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 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 Management Centre has the same status as the

official 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, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: Avenue Marnix 17, B-1000 Brussels

© 2009 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 23913:2009: E

worldwide for CEN national Members.
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SIST EN ISO 23913:2009
EN ISO 23913:2009 (E)
Contents Page

Foreword ..............................................................................................................................................................3

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SIST EN ISO 23913:2009
EN ISO 23913:2009 (E)
Foreword

The text of ISO 23913:2006 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 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 publication 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] 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, 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 by CEN as a EN ISO 23913:2009 without any modification.

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SIST EN ISO 23913:2009
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SIST EN ISO 23913:2009
INTERNATIONAL ISO
STANDARD 23913
First edition
2006-05-15
Water quality — Determination of
chromium(VI) — Method using flow
analysis (FIA and CFA) and spectrometric
detection
Qualité de l'eau — Dosage du chrome(VI) — Méthode par analyse en
flux (FIA et CFA) et détection spectrométrique
Reference number
ISO 23913:2006(E)
ISO 2006
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SIST EN ISO 23913:2009
ISO 23913:2006(E)
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© ISO 2006

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ii © ISO 2006 – All rights reserved
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SIST EN ISO 23913:2009
ISO 23913:2006(E)
Contents Page

Foreword............................................................................................................................................................ iv

Introduction ........................................................................................................................................................ v

1 Scope ..................................................................................................................................................... 1

2 Normative references ........................................................................................................................... 1

3 Principle................................................................................................................................................. 1

4 Interferences ......................................................................................................................................... 2

5 Reagents................................................................................................................................................ 2

6 Apparatus .............................................................................................................................................. 5

7 Sampling and sample preparation...................................................................................................... 6

8 Procedure .............................................................................................................................................. 6

9 Determination........................................................................................................................................ 7

10 Expression of results ........................................................................................................................... 8

11 Test report ............................................................................................................................................. 8

Annex A (informative) Examples of flow analysis systems for the determination of chromium(VI)......... 9

Annex B (informative) Performance characteristics..................................................................................... 12

Bibliography ..................................................................................................................................................... 14

© ISO 2006 – All rights reserved iii
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SIST EN ISO 23913:2009
ISO 23913:2006(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 23913 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical,

chemical and biochemical methods.
iv © ISO 2006 – All rights reserved
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SIST EN ISO 23913:2009
ISO 23913:2006(E)
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.
[1], [2]

Analysis can be performed by flow injection analysis (FIA) and 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 sample

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.
© ISO 2006 – All rights reserved v
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SIST EN ISO 23913:2009
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SIST EN ISO 23913:2009
INTERNATIONAL STANDARD ISO 23913:2006(E)
Water quality — Determination of chromium(VI) — Method
using flow analysis (FIA and CFA) and spectrometric detection

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

are carried out by suitably qualified staff.
1 Scope

This International Standard specifies flow injection analysis (FIA) and 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 µg/l to 200 µg/l and 200 µg/l to 2 000 µg/l for surface water, leachates and waste water.

CFA: 2 µg/l to 20 µg/l and 20 µg/l to 200 µg/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 salinity 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 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 — Part 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).

© ISO 2006 – All rights reserved 1
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SIST EN ISO 23913:2009
ISO 23913:2006(E)
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 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 significant 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 the 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, H SO ) until the above mentioned test leads to sufficient results.

2 4

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 solution 5.10 for feeding line “R2” in Figures A.1 to A.3. Subtract the result of this measurement y

from 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 checked

(see 8.3).
5.2 Sulfuric acid, ρ(H SO ) = 1,84 g/ml.
2 4
5.3 Orthophosphoric acid, ρ(H PO ) = 1,71 g/ml.
3 4

5.4 Surfactant solution, aqueous polyethylene glycol dodecyl ether, [HO-(CH -CH O) C H ], with a

2 2 n 12 21
mass fraction of 30 %.
2 © ISO 2006 – All rights reserved
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SIST EN ISO 23913:2009
ISO 23913:2006(E)
5.5 Acid mixtures.
5.5.1 Acid 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 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, C H N O.
13 14 4
5.7 Acetone, C H O.
3 6
5.8 1-Propanol, C H O.
3 8
5.9 Potassium dichromate, K Cr O .
2 2 7
5.10 Diphenylcarbazide solution, (R2 in Figures A.1 to A.3).

Dissolve in a 250 ml beaker 0,43 g of 1,5-diphenylcarbazide (5.6) in 9 ml of acetone (5.7) and 9 ml of

1-propanol (5.8). Add 125 ml of 1-propanol (5.8).Transfer the mixture to a 250 ml volumetric flask, and make

up to volume with water (5.1).

The solution is stable for up to 1 week if stored in a brown glass bottle at 2 °C to 6 °C.

If precipitation occurs, filter the solution.

NOTE The use of a mixture of acetone and 1-propanol permits the redissolving of precipitates of

1,5-diphenylcarbazide occurring on cooling. In the literature, several solvents (acetone, 1-propanol, 2-propanol, ethanol, in

combination with water) are proposed for preparing the diphenylcarbazide solution. These alternatives are also applicable,

provided the solutions are stable enough and contain the same concentration of 1,5-diphenylcarbazide (5.6) as given

in 5.10.

Degas carefully all reagent solutions for the FIA determinations before use, e.g. by vacuum filtration.

5.11 Carrier solution for FIA systems, (C in Figure A.1).
Use water (5.1).

Carrier and samples should have identical acidity. For unpreserved samples, this means that water should be

used as a carrier.
...

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