EN ISO 5536:2013

Milk fat products - Determination of water content - Karl Fischer method (ISO 5536:2009)

ISO 5536|IDF 23:2009 specifies a method for the determination of the water content of milk fat products by the Karl Fischer method.
The method is applicable to butteroil (anhydrous butteroil, anhydrous butterfat, anhydrous milk fat) with a water content not exceeding 1,0 % mass fraction.

Milchfett-Erzeugnisse - Bestimmung des Wassergehaltes - Karl-Fischer-Verfahren (ISO 5536:2009)

Diese Internationale Norm legt ein Verfahren zur Bestimmung des Wassergehaltes von Milchfett-Erzeugnissen unter Anwendung des Karl Fischer (KF )Verfahrens fest.
Das Verfahren ist auf Butterfett (wasserfreies Butterfett, wasserfreies Butterschmalz, wasserfreies Milchfett) mit einem Wassergehalt von höchstens 1,0 % (Massenanteil) anwendbar.

Produits à base de matière grasse laitière - Détermination de la teneur en eau - Méthode de Karl Fischer (ISO 5536:2009)

L'ISO 5536|FIL 23:2009 spécifie une méthode de détermination de la teneur en eau des produits à base de matière grasse laitière par la méthode de Karl Fischer.
Cette méthode s'applique à l'huile de beurre (huile de beurre anhydre, matière grasse butyrique anhydre, matière grasse laitière anhydre) dont la teneur en eau ne dépasse pas 1,0 % (fraction massique).

Proizvodi na osnovi mlečnih maščob - Določevanje vode - Metoda po Karlu Fischerju (ISO 5536:2009)

Ta mednarodni standard določa metodo za določevanje količine vode v mlečnih maščobah z metodo po Karl Fischerju (KF). Ta metoda se uporablja za masleno olje (anhidridno masleno olje, anhidridna maslena maščoba, anhidridna mlečna maščoba) z vsebnostjo vode, ki ne presega 1,0 % masnega deleža.

General Information

• Status: Published
• Publication Date: 28-May-2013
• Withdrawal Date: 29-Nov-2013
• ICS: 67.100.10 - Milk and processed milk products
• Technical Committee: CEN/TC 302 - Milk and milk products - Methods of sampling and analysis
• Drafting Committee: CEN/TC 302 - Milk and milk products - Methods of sampling and analysis
• Current Stage: 6060 - Definitive text made available (DAV) - Publishing
• Start Date: 29-May-2013
• Due Date: 23-Apr-2014
• Completion Date: 29-May-2013
• Ref Project: SIST EN ISO 5536:2013 - Milk fat products - Determination of water content - Karl Fischer method (ISO 5536:2009)

Overview

EN ISO 5536:2013 (ISO 5536:2009) specifies the Karl Fischer (KF) method for determining the water content of milk fat products, specifically applicable to butteroil / anhydrous milk fat with water content up to 1.0 % (mass fraction). Adopted by CEN from ISO/IDF, this standard defines reagents, apparatus, procedure and calculation steps for accurate volumetric KF titration of milk fat matrices.

Key topics and requirements

• Scope: Analysis of milk fat products (butteroil/anhydrous butterfat) with ≤ 1.0 % water.
• Principle: Direct volumetric titration of the test sample with a commercially available, pyridine‑free two‑component KF reagent at approximately 40 °C; water content calculated from reagent volume used.
• Reagents:
  • Two‑component pyridine‑free Karl Fischer reagent (or one‑component titration reagent with methanol as solvent).
  • Titration component with water equivalent ≈ 2 mg/ml.
  • 1‑Octanol and methanol (methanol water content ≤ 0.05 %).
  • Water standard (w = 10 mg/g) for calibration of the titration component.
• Working medium: Mix equal volumes of solvent component and 1‑octanol (1+1) in the titration vessel (~30 ml recommended).
• Apparatus:
  • Automatic volumetric KF titrator with 5 ml (preferred) or 10 ml burette, double‑jacketed titration vessel and water bath for controlled ~40 °C titrations.
  • Analytical balance (readability 0.1 mg) and disposable syringes (5 ml or 10 ml).
• Key procedural controls:
  • Determine KF apparatus drift daily (titration without sample) and express drift in mL/min or mg/min.
  • Establish water equivalent of titration component via five replicate titrations using the water standard; report mean to three decimal places.
  • Shut-off criterion: typically a 10 s stop delay or stop drift slightly above measured drift.
  • Sample preparation: mix sample thoroughly at 35–40 °C to disperse water; typical test portion ≈ 5 g. Replicates recommended for accuracy.

Applications and users

• Who uses it: dairy quality control laboratories, butteroil producers, food testing laboratories, regulatory agencies and research institutes concerned with milk fat product quality and specification compliance.
• Why use it: precise, standardized measurement of low-level water content for product shelf-life assessment, quality control, specification verification, trade and regulatory compliance.

Related standards

• ISO 707 | IDF 50 (recommended sampling method for milk and milk products) is referenced for sampling practices.
• CEN adoption: EN ISO 5536:2013 is the CEN-endorsed version of ISO 5536:2009.

Keywords: EN ISO 5536:2013, ISO 5536:2009, Karl Fischer, water content, milk fat products, butteroil, KF titration, anhydrous milk fat, dairy laboratory.

Standards Content (Sample)

SLOVENSKI STANDARD
01-september-2013
3URL]YRGLQDRVQRYLPOHþQLKPDãþRE'RORþHYDQMHYRGH0HWRGDSR.DUOX
)LVFKHUMX,62
Milk fat products - Determination of water content - Karl Fischer method (ISO 5536:2009)
Milchfett-Erzeugnisse - Bestimmung des Wassergehaltes - Karl-Fischer-Verfahren (ISO
5536:2009)
Produits à base de matière grasse laitière - Détermination de la teneur en eau - Méthode
de Karl Fischer (ISO 5536:2009)
Ta slovenski standard je istoveten z: EN ISO 5536:2013
ICS:
67.100.10 0OHNRLQSUHGHODQLPOHþQL Milk and processed milk
SURL]YRGL products
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EUROPEAN STANDARD
EN ISO 5536
NORME EUROPÉENNE
EUROPÄISCHE NORM
May 2013
ICS 67.100.10
English Version
Milk fat products - Determination of water content - Karl Fischer
method (ISO 5536:2009)
Produits à base de matière grasse laitière - Détermination Milchfett-Erzeugnisse - Bestimmung des Wassergehaltes -
de la teneur en eau - Méthode de Karl Fischer (ISO Karl-Fischer-Verfahren (ISO 5536:2009)
5536:2009)
This European Standard was approved by CEN on 16 May 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 5536:2013: E
worldwide for CEN national Members.

Contents Page
Foreword .3

Foreword
The text of ISO 5536:2009 has been prepared by Technical Committee ISO/TC 34 “Food products” of the
International Organization for Standardization (ISO) and has been taken over as EN ISO 5536:2013 by
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 November 2013, and conflicting national standards shall be withdrawn
at the latest by November 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 5536:2009 has been approved by CEN as EN ISO 5536:2013 without any modification.

INTERNATIONAL ISO
STANDARD 5536
IDF
Second edition
2009-11-15
Milk fat products — Determination of
water content — Karl Fischer method
Produits à base de matière grasse laitière — Détermination de la teneur
en eau — Méthode de Karl Fischer

Reference numbers
ISO 5536:2009(E)
IDF 23:2009(E)
©
ISO and IDF 2009
ISO 5536:2009(E)
IDF 23:2009(E)
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ii © ISO and IDF 2009 – All rights reserved

ISO 5536:2009(E)
IDF 23:2009(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
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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 5536⎪IDF 23 was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 5,
Milk and milk products, and the International Dairy Federation (IDF). It is being published jointly by ISO and
IDF.
This second edition of ISO 5536⎪IDF 23 cancels and replaces the first edition (ISO 5536⎪IDF 23:2002), which
has been technically revised.
ISO 5536:2009(E)
IDF 23:2009(E)
Foreword
IDF (the International Dairy Federation) is a non-profit organization representing the dairy sector worldwide.
IDF membership comprises National Committees in every member country as well as regional dairy
associations having signed a formal agreement on cooperation with IDF. All members of IDF have the right to
be represented on the IDF Standing Committees carrying out the technical work. IDF collaborates with ISO in
the development of standard methods of analysis and sampling for milk and milk products.
The main task of Standing Committees is to prepare International Standards. Draft International Standards
adopted by the Standing Committees are circulated to the National Committees for endorsement prior to
publication as an International Standard. Publication as an International Standard requires approval by at least
50 % of IDF National Committees casting a vote.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. IDF shall not be held responsible for identifying any or all such patent rights.
International Standard ISO 5536⎪IDF 23 was prepared by Technical Committee ISO/TC 34, Food products,
Subcommittee SC 5, Milk and milk products and the International Dairy Federation (IDF). It is being published
jointly by ISO and IDF.
All work was carried out by the Joint ISO-IDF Action Team on Water of the Standing Committee on Main
components in milk under the aegis of its project leader, Prof. Dr. H.-D. Isengard (DE).
This edition of ISO 5536⎪IDF 23 cancels and replaces ISO 5536⎪IDF 23:2002, which has been technically
revised.
iv © ISO and IDF 2009 – All rights reserved

ISO 5536:2009(E)
INTERNATIONAL STANDARD
IDF 23:2009(E)
Milk fat products — Determination of water content — Karl
Fischer method
1 Scope
This International Standard specifies a method for the determination of the water content of milk fat products
by the Karl Fischer (KF) method.
The method is applicable to butteroil (anhydrous butteroil, anhydrous butterfat, anhydrous milk fat) with a
water content not exceeding 1,0 % mass fraction.
2 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
2.1
water content of milk fat products
w
HO
mass fraction of water determined by the procedure specified in this International Standard
NOTE The water content is expressed as a percentage mass fraction.
3 Principle
The test sample is directly titrated with a commercially available two-component Karl Fischer reagent at a
temperature of approximately 40 °C. The water content is calculated from the amount of reagent used.
4 Reagents
Use only reagents of recognized analytical grade, unless otherwise specified, and distilled or demineralized
water or water of equivalent purity.
Avoid absorption of moisture from the environment.
4.1 Karl Fischer (KF) reagent, a commercially available pyridine-free two-component reagent consisting of
a titration component (4.2) and a solvent component.
Alternatively, a pyridine-free one-component KF reagent consisting solely of a titration component (4.2) can
also be used, in which case, methanol (4.6) is used as the solvent component.
4.2 Titration component.
The titration component of the KF reagent (4.1) shall have a water equivalent of approximately 2 mg/ml.
4.3 1-Octanol (C H OH)
8 17
ISO 5536:2009(E)
IDF 23:2009(E)
4.4 Working medium.
Prepare the working medium by mixing equal volumes of the solvent component of the KF reagent (4.1) and
1-octanol (4.3) (1+1) directly in the titration vessel of the KF apparatus (5.1).
4.5 Water standard, w = 10 mg/g.
H O
For the determination of the water equivalent of the titration component, use a commercially available liquid
water standard.
4.6 Methanol (CH OH), with a water content of not more than 0,05 %
...