Milk and milk products - Determination of nitrate and nitrite contents - Part 3: Method using cadmium reduction and flow injection analysis with in-line dialysis (Routine method) (ISO 14673-3:2004)

ISO 14673-3|IDF 189-3:2004 specifies a routine method for the determination of the nitrate and nitrite contents of milk and milk products by cadmium reduction and flow injection analysis (FIA). The method is applicable to hard, semi-hard and soft cheeses of various ages, and processed cheese. The detection limits of the method are 0,5 mg of nitrate ions per kilogram and 1,0 mg of nitrite ions per kilogram, respectively.
The method is also applicable to whey powder, milk powder and milk-based infant food.

Milch und Milchprodukte - Bestimmung des Nitrat- und Nitritgehaltes - Teil 3: Verfahren mit Cadmiumreduktion und Fließinjektionsanalyse mit In-line-Dialyse (Routineverfahren) (ISO14673-3:2004)

Dieser Teil von ISO 14673|IDF 189 legt ein Verfahren zur Bestimmung des Nitrat- und Nitritgehaltes von Milch und Milchprodukten durch Cadmiumreduktion und Fließinjektionsanalyse (FIA) fest. Das Verfahren gilt für Hart-, Schnitt- und Weichkäse unterschiedlichen Alters und für Schmelzkäse. Die Nachweisgrenzen des Verfahrens liegen bei 0,5 mg Nitrat-Ionen je Kilogramm und bei 1,0 mg Nitrit-Ionen je Kilogramm.
Das Verfahren gilt auch für Molkenpulver, Milchpulver und Säuglings- und Kleinkindernahrung auf Milchbasis.
ANMERKUNG 1   Das Verfahren ähnelt sehr dem in [2] beschriebenen FIA-Verfahren zur Bestimmung von Nitrat und Nitrit in Milch und flüssigen Molkereiprodukten. Um die Analyse von Käse zu ermöglichen und um eine ausreichende Empfindlichkeit für die Bestimmung geringer Nitritkonzentrationen in Käse und Säuglingsnahrung zu erreichen, wurden Anpassungen vorgenommen.
ANMERKUNG 2   Bei der Nitrit- und Nitratbestimmung mit Cadmiumreduktion wird die gleiche Farbreaktion verwendet, wie sie in ISO 14673-1|IDF 189 beschrieben ist.

Lait et produits laitiers - Détermination des teneurs en nitrates et en nitrites - Partie 3: Méthode par réduction au cadmium et d'analyse par injection de flux avec dialyse en ligne (Méthode de routine) (ISO 14673-3:2004)

L'ISO 14673-3|FIL 189-3:2004 spécifie une méthode de routine pour la détermination des teneurs en nitrates et nitrites dans le fromage par réduction au cadmium et analyse par injection de flux. La méthode s'applique aux fromages à pâte dure, aux fromages à pâte semi-dure, aux fromages à pâte molle à longueur d'affinage variable ainsi qu'aux fromages fondus. Les limites de détection de la méthode sont de 0,5 mg d'ions nitrate par kilogramme et de 1,0 mg d'ions nitrite par kilogramme.
Cette méthode s'est également avérée adaptée pour la poudre de petit-lait, le lait en poudre et les aliments à base de lait pour bébés.

Mleko in mlečni proizvodi - Določevanje nitratov in nitritov - 3. del: Metoda z uporabo redukcije s kadmijem in pretočno analizo z in-line dializo (ISO 14673-3:2004)

General Information

Status
Published
Publication Date
30-Apr-2004
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
01-May-2004
Due Date
01-May-2004
Completion Date
01-May-2004

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SLOVENSKI STANDARD
SIST EN ISO 14673-3:2004
01-maj-2004
0OHNRLQPOHþQLSURL]YRGL'RORþHYDQMHQLWUDWRYLQQLWULWRYGHO0HWRGD]
XSRUDERUHGXNFLMHVNDGPLMHPLQSUHWRþQRDQDOL]R]LQOLQHGLDOL]R ,62

Milk and milk products - Determination of nitrate and nitrite contents - Part 3: Method
using cadmium reduction and flow injection analysis with in-line dialysis (Routine
method) (ISO 14673-3:2004)
Milch und Milchprodukte - Bestimmung des Nitrat- und Nitritgehaltes - Teil 3: Verfahren
mit Cadmiumreduktion und Fließinjektionsanalyse mit In-line-Dialyse (Routineverfahren)
(ISO14673-3:2004)
Lait et produits laitiers - Détermination des teneurs en nitrates et en nitrites - Partie 3:
Méthode par réduction au cadmium et d'analyse par injection de flux avec dialyse en
ligne (Méthode de routine) (ISO 14673-3:2004)
Ta slovenski standard je istoveten z: EN ISO 14673-3:2004
ICS:
67.100.01 0OHNRLQPOHþQLSURL]YRGLQD Milk and milk products in
VSORãQR general
SIST EN ISO 14673-3:2004 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 14673-3:2004

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SIST EN ISO 14673-3:2004
EUROPEAN STANDARD
EN ISO 14673-3
NORME EUROPÉENNE
EUROPÄISCHE NORM
February 2004
ICS 67.100.10 Supersedes EN ISO 14673-3:2001
English version
Milk and milk products - Determination of nitrate and nitrite
contents - Part 3: Method using cadmium reduction and flow
injection analysis with in-line dialysis (Routine method) (ISO
14673-3:2004)
Lait et produits laitiers - Détermination des teneurs en Milch und Milchprodukte - Bestimmung des Nitrat- und
nitrates et en nitrites - Partie 3: Méthode par réduction au Nitritgehaltes - Teil 3: Verfahren mit Cadmiumreduktion
cadmium et d'analyse par injection de flux avec dialyse en und Fließinjektionsanalyse mit In-line-Dialyse
ligne (Méthode de routine) (ISO 14673-3:2004) (Routineverfahren) (ISO14673-3:2004)
This European Standard was approved by CEN on 2 February 2004.
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 Central Secretariat 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 Central Secretariat has the same status as the official
versions.
CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,
Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,
Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36  B-1050 Brussels
© 2004 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 14673-3:2004: E
worldwide for CEN national Members.

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SIST EN ISO 14673-3:2004
EN ISO 14673-3:2004 (E)
CORRECTED  2004-03-03
Foreword
This document (EN ISO 14673-3:2004) has been prepared by Technical Committee ISO/TC 34
"Agricultural food products" in collaboration with Technical Committee CEN/TC 302 "Milk and
milk products - Methods of sampling and analysis", the secretariat of which is held by NEN.
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 August 2004, and conflicting national
standards shall be withdrawn at the latest by August 2004.
This document supersedes EN ISO 14673-3:2001.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of
the following countries are bound to implement this European Standard: Austria, Belgium,
Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary,
Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,
Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
Endorsement notice
The text of ISO 14673-3:2004 has been approved by CEN as EN ISO 14673-3:2004 without any
modifications.
2

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SIST EN ISO 14673-3:2004



INTERNATIONAL ISO
STANDARD 14673-3
IDF
189-3
Second edition
2004-02-01


Milk and milk products — Determination
of nitrate and nitrite contents —
Part 3:
Method using cadmium reduction and
flow injection analysis with in-line
dialysis (Routine method)
Lait et produits laitiers — Détermination des teneurs en nitrates et en
nitrites —
Partie 3: Méthode par réduction au cadmium et d'analyse par injection
de flux avec dialyse en ligne (Méthode de routine)




Reference numbers
ISO 14673-3:2004(E)
IDF 189-3:2004(E)
©
ISO and IDF 2004

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SIST EN ISO 14673-3:2004
ISO 14673-3:2004(E)
IDF 189-3:2004(E)
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©  ISO and IDF 2004
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 or IDF at the respective
address below.
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Tel. + 41 22 749 01 11 Tel. + 32 2 733 98 88
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Web www.iso.org Web www.fil-idf.org
Published in Switzerland

ii © ISO and IDF 2004 – All rights reserved

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SIST EN ISO 14673-3:2004
ISO 14673-3:2004(E)
IDF 189-3:2004(E)
Contents Page
Foreword. iv
1 Scope. 1
2 Normative references . 1
3 Terms and definitions. 1
4 Principle . 2
5 Reagents . 2
6 Apparatus. 3
7 Sampling . 5
8 Preparation of test sample. 5
8.1 Cheese. 5
9 Procedure. 6
9.1 Checking the reducing capacity of the cadmium column . 6
9.2 Regeneration of the cadmium column. 6
9.3 Test portion . 6
9.4 Extraction. 6
9.5 Determination of nitrite content . 7
9.6 Determination of nitrate content . 7
10 Calculation and expression of results . 7
10.1 Nitrite content. 7
10.2 Nitrate content. 8
11 Precision . 8
11.1 General. 8
11.2 Nitrite content. 8
11.3 Nitrate content. 9
12 Test report. 9
Bibliography . 10

© ISO and IDF 2004 – All rights reserved iii

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SIST EN ISO 14673-3:2004
ISO 14673-3:2004(E)
IDF 189-3:2004(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 14673-3IDF 189-3 was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee
SC 5, Milk and milk products, and the International Dairy Federation (IDF), in collaboration with AOAC
International. It is being published jointly by ISO and IDF and separately by AOAC International.
This second edition cancels and replaces the first edition (ISO 14673-3IDF 189-3:2001), of which it
constitutes a minor revision.
ISO 14673IDF 189 consists of the following parts, under the general title Milk and milk products —
Determination of nitrate and nitrite contents:
— Part 1: Method using cadmium reduction and spectrometry
— Part 2: Method using segmented flow analysis (Routine method)
— Part 3: Method using cadmium reduction and flow injection analysis with in-line dialysis (Routine method)

iv © ISO and IDF 2004 – All rights reserved

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SIST EN ISO 14673-3:2004
ISO 14673-3:2004(E)
IDF 189-3:2004(E)
Foreword
IDF (the International Dairy Federation) is a worldwide federation of the dairy sector with a National
Committee in every member country. Every National Committee has the right to be represented on the IDF
Standing Committees carrying out the technical work. IDF collaborates with ISO and AOAC International in
the development of standard methods of analysis and sampling for milk and milk products.
Draft International Standards adopted by the Action Teams and Standing Committees are circulated to the
National Committees for voting. Publication as an International Standard requires approval by at least 50 % of
the National Committees casting a vote.
ISO 14673-3IDF 189-3 was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee
SC 5, Milk and milk products, and the International Dairy Federation (IDF), in collaboration with AOAC
International. It is being published jointly by ISO and IDF and separately by AOAC International.
All work was carried out by the Joint ISO/IDF/AOAC Action Team, Minerals and minor compounds, of the
Standing Committee on Minor components characterization of physical properties, under the aegis of its
project leader, Mr G. Bråthen (NO).
This second edition, together with ISO 14673-1IDF 189-1 and ISO 14673-2IDF 189-2, cancels and replaces
IDF 84A:1984, IDF 95A:1982, IDF 96A:1987, IDF 97A:1985 and IDF 120:1984, which have been technically
revised.

© ISO and IDF 2004 – All rights reserved v

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SIST EN ISO 14673-3:2004

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SIST EN ISO 14673-3:2004
ISO 14673-3:2004(E)
INTERNATIONAL STANDARD
IDF 189-3:2004(E)

Milk and milk products — Determination of nitrate and nitrite
contents —
Part 3:
Method using cadmium reduction and flow injection analysis
with in-line dialysis (Routine method)
WARNING — The use of this International Standard may involve hazardous materials, operations and
equipment. This standard does not purport to address all the safety problems associated with its use.
It is the responsibility of the user of this standard to establish safety and health practices and
determine the applicability of regulatory limitations prior to use.
1 Scope
This part of ISO 14673IDF 189 specifies a routine method for the determination of the nitrate and nitrite
contents of milk and milk products by cadmium reduction and flow injection analysis (FIA). The method is
applicable to hard, semi-hard and soft cheeses of various ages, and processed cheese. The detection limits of
the method are 0,5 mg of nitrate ions per kilogram and 1,0 mg of nitrite ions per kilogram.
The method is also applicable to whey powder, milk powder and milk-based infant food.
NOTE 1 The method closely resembles the FIA method described in reference [2] for the determination of nitrate and
nitrite in milk and fluid dairy products. Adaptations were made to allow for the analysis of cheese and to obtain sufficient
sensitivity for the determination of low levels of nitrite in cheese and milk-based infant foods.
NOTE 2 For determination of nitrite and nitrate following cadmium reduction, use is made of the same colour reaction
as described in ISO 14673-1IDF 189-1.
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 1042, Laboratory glassware — One-mark volumetric flasks
ISO 14673-1IDF 189-1, Milk and milk products — Determination of nitrate and nitrite contents — Part 1:
Method using cadmium reduction and spectrometry
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
nitrate content
mass fraction of nitrate determined by the procedure specified in this part of ISO 14673IDF 189

NOTE The nitrate content is expressed as the mass in milligrams of nitrate ions (NO ) per kilogram of product.
3
© ISO and IDF 2004 – All rights reserved 1

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SIST EN ISO 14673-3:2004
ISO 14673-3:2004(E)
IDF 189-3:2004(E)
3.2
nitrite content
mass fraction of nitrite determined by the procedure specified in this part of ISO 14673IDF 189

NOTE The nitrite content is expressed as the mass in milligrams of nitrite ions (NO ) per kilogram of product.
2
4 Principle
4.1 A test portion is suspended in a warm extraction buffer solution. Fat is separated by centrifuging and
rapid cooling. Analyses are made of small portions of the de-fatted solution by flow injection analysis (FIA). In-
line dialysis is used to remove protein and remaining fat. The nitrate ions are reduced to nitrite ions by
cadmium. The nitrite ions are reacted with sulfanilamide and N-1-naphthyl ethylenediamine dihydrochloride to
give a red-coloured azo dye. The colour is measured in a flow cell at maximum absorption of the dye
...

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