SIST-TS CEN ISO/TS 17764-1:2007
(Main)Animal feeding stuffs - Determination of the content of fatty acids - Part 1: Preparation of methyl esters (ISO/TS 17764-1:2002)
Animal feeding stuffs - Determination of the content of fatty acids - Part 1: Preparation of methyl esters (ISO/TS 17764-1:2002)
ISO/TS 17764-1:2002 specifies two methods for preparing the methyl esters of fatty acids of animal and vegetable fats, oils and fatty acid mixtures for raw materials for compound animal feeds, and fatty acids originating from fat extracts of animal feeding stuffs, including fats and fatty acid mixtures containing butyric acid.
The general method, the boron trifluoride (BF3) method is concerned with the preparation of methyl esters of fatty acids with six or more C atoms, originating from fats, oils and free fatty acids.
The KOH/HCl method is concerned with the preparation of methyl esters of fatty acids with four or more C atoms. This method can also be used for the quantitative determination of fatty acids with a chain length shorter than 10 C atoms in free fatty acid mixtures.
The methyl esters produced can be used for gas-liquid chromatography (GLC).
Unsaponifiable materials are not removed and can, when present in considerable amounts, interfere with the chromatographic analysis.
ISO/TS 17764-2:2002 describes the application of gas chromatography with capillary columns and flame ionization detection for the determination of the content of fatty acids in a fat by making use of the methyl esters of the fatty acids obtained in accordance with the methods specified in ISO/TS 17764-1:2002.
Futtermittel - Bestimmung des Gehaltes an Fettsäuren - Teil 1: Vorbereitung von Methylestern (ISO/TS 17764-1:2002)
Aliments des animaux - Détermination de la teneur en acides gras - Partie 1: Préparation des esters méthyliques (ISO/TS 17764-1:2002)
Krma - Določevanje maščobnih kislin - 1. del: Priprava metil estrov (ISO/TS 17764-1:2002)
General Information
- Status
- Published
- Publication Date
- 28-Feb-2007
- Technical Committee
- KŽP - Agricultural food products
- Current Stage
- 6060 - National Implementation/Publication (Adopted Project)
- Start Date
- 01-Mar-2007
- Due Date
- 01-Mar-2007
- Completion Date
- 01-Mar-2007
Overview
CEN ISO/TS 17764-1:2006 (ISO/TS 17764-1:2002) defines validated laboratory procedures for preparing fatty acid methyl esters (FAMEs) from animal and vegetable fats, oils and fatty acid mixtures in animal feeding stuffs. The methyl esters produced are intended for subsequent analysis by gas‑liquid chromatography (GLC/GC) to quantify individual fatty acids and the total elutable fatty acids in feed raw materials and fat extracts.
Key topics and technical requirements
- Two complementary methylation routes:
- BF3 (boron trifluoride) method - targeted at fatty acids with six or more carbon atoms (C6+); involves saponification with methanolic NaOH followed by methylation with a commercial BF3/methanol complex.
- KOH/HCl (KOH–HCl / potassium methanolate) method - suitable for fatty acids with four or more carbon atoms (C4+); uses potassium methanolate (transesterification) and HCl/methanol for free fatty acids. This method can quantify short‑chain fatty acids (< C10) in free fatty acid mixtures.
- Reagents, apparatus and safety:
- Use analytical‑grade solvents (n‑hexane, n‑heptane, n‑pentane), anhydrous methanol, saturated NaCl, and anhydrous Na2SO4.
- Heptadecanoic acid (C17:0) is used as an internal standard (≈20% of test portion mass).
- BF3 is toxic - methylation with BF3 must be performed in a ventilated hood; check reagents for GC‑interfering peaks (BF3 solutions can produce peaks near C20–C22).
- Sample preparation and extraction:
- Fat extraction and sample handling follow ISO 6492 and ISO 661 guidance (category‑based extraction, solvent removal, drying).
- Unsaponifiable materials are not removed by these procedures and, when abundant, can interfere with chromatographic analysis.
- Output: Prepared FAME solutions at concentrations suitable for GC analysis; dilution recommendations for cold on‑column injection are provided.
Applications and users
- Practical uses:
- Routine laboratory determination of fatty acid profiles in raw materials for compound feeds, feed ingredients, and fat extracts from animal feeding stuffs.
- Preparation of FAMEs for GC with capillary columns and flame ionization detection (see Part 2).
- Typical users:
- Feed testing laboratories, quality control teams in feed manufacturing, research laboratories studying feed lipid composition, regulatory and certification bodies performing compositional analysis.
Related standards
- ISO/TS 17764-2:2002 - Gas chromatographic method for fatty acid determination using the FAMEs produced per Part 1.
- ISO 6492:1999 - Fat content determination and extraction guidance.
- ISO 661 - Sample preparation for fats and oils.
- ISO 3696 - Water quality for analytical use (reagent water).
Keywords: CEN ISO/TS 17764-1:2006, animal feeding stuffs, fatty acid methyl esters, FAMEs, gas‑liquid chromatography, BF3 methylation, potassium methanolate, sample preparation, heptadecanoic acid, unsaponifiables.
Frequently Asked Questions
SIST-TS CEN ISO/TS 17764-1:2007 is a technical specification published by the Slovenian Institute for Standardization (SIST). Its full title is "Animal feeding stuffs - Determination of the content of fatty acids - Part 1: Preparation of methyl esters (ISO/TS 17764-1:2002)". This standard covers: ISO/TS 17764-1:2002 specifies two methods for preparing the methyl esters of fatty acids of animal and vegetable fats, oils and fatty acid mixtures for raw materials for compound animal feeds, and fatty acids originating from fat extracts of animal feeding stuffs, including fats and fatty acid mixtures containing butyric acid. The general method, the boron trifluoride (BF3) method is concerned with the preparation of methyl esters of fatty acids with six or more C atoms, originating from fats, oils and free fatty acids. The KOH/HCl method is concerned with the preparation of methyl esters of fatty acids with four or more C atoms. This method can also be used for the quantitative determination of fatty acids with a chain length shorter than 10 C atoms in free fatty acid mixtures. The methyl esters produced can be used for gas-liquid chromatography (GLC). Unsaponifiable materials are not removed and can, when present in considerable amounts, interfere with the chromatographic analysis. ISO/TS 17764-2:2002 describes the application of gas chromatography with capillary columns and flame ionization detection for the determination of the content of fatty acids in a fat by making use of the methyl esters of the fatty acids obtained in accordance with the methods specified in ISO/TS 17764-1:2002.
ISO/TS 17764-1:2002 specifies two methods for preparing the methyl esters of fatty acids of animal and vegetable fats, oils and fatty acid mixtures for raw materials for compound animal feeds, and fatty acids originating from fat extracts of animal feeding stuffs, including fats and fatty acid mixtures containing butyric acid. The general method, the boron trifluoride (BF3) method is concerned with the preparation of methyl esters of fatty acids with six or more C atoms, originating from fats, oils and free fatty acids. The KOH/HCl method is concerned with the preparation of methyl esters of fatty acids with four or more C atoms. This method can also be used for the quantitative determination of fatty acids with a chain length shorter than 10 C atoms in free fatty acid mixtures. The methyl esters produced can be used for gas-liquid chromatography (GLC). Unsaponifiable materials are not removed and can, when present in considerable amounts, interfere with the chromatographic analysis. ISO/TS 17764-2:2002 describes the application of gas chromatography with capillary columns and flame ionization detection for the determination of the content of fatty acids in a fat by making use of the methyl esters of the fatty acids obtained in accordance with the methods specified in ISO/TS 17764-1:2002.
SIST-TS CEN ISO/TS 17764-1:2007 is classified under the following ICS (International Classification for Standards) categories: 65.120 - Animal feeding stuffs. The ICS classification helps identify the subject area and facilitates finding related standards.
SIST-TS CEN ISO/TS 17764-1:2007 is available in PDF format for immediate download after purchase. The document can be added to your cart and obtained through the secure checkout process. Digital delivery ensures instant access to the complete standard document.
Standards Content (Sample)
SLOVENSKI STANDARD
01-marec-2007
.UPD'RORþHYDQMHPDãþREQLKNLVOLQGHO3ULSUDYDPHWLOHVWURY,6276
Animal feeding stuffs - Determination of the content of fatty acids - Part 1: Preparation of
methyl esters (ISO/TS 17764-1:2002)
Futtermittel - Bestimmung des Gehaltes an Fettsäuren - Teil 1: Vorbereitung von
Methylestern (ISO/TS 17764-1:2002)
Aliments des animaux - Détermination de la teneur en acides gras - Partie 1: Préparation
des esters méthyliques (ISO/TS 17764-1:2002)
Ta slovenski standard je istoveten z: CEN ISO/TS 17764-1:2006
ICS:
65.120 Krmila Animal feeding stuffs
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
TECHNICAL SPECIFICATION
CEN ISO/TS 17764-1
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
October 2006
ICS 65.120
English Version
Animal feeding stuffs - Determination of the content of fatty
acids - Part 1: Preparation of methyl esters (ISO/TS 17764-
1:2002)
Aliments des animaux - Détermination de la teneur en Futtermittel - Bestimmung des Gehaltes an Fettsäuren -
acides gras - Partie 1: Préparation des esters méthyliques Teil 1: Vorbereitung von Methylestern (ISO/TS 17764-
(ISO/TS 17764-1:2002) 1:2002)
This Technical Specification (CEN/TS) was approved by CEN on 13 February 2006 for provisional application.
The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to submit their
comments, particularly on the question whether the CEN/TS can be converted into a European Standard.
CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS available
promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the CEN/TS)
until the final decision about the possible conversion of the CEN/TS into an EN is reached.
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, Romania,
Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
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© 2006 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN ISO/TS 17764-1:2006: E
worldwide for CEN national Members.
Foreword
This document (CEN ISO/TS 17764-1:2006) has been prepared by Technical Committee
CEN/TC 327 "Animal feeding stuffs - Methods of sampling and analysis", the secretariat of which
is held by NEN, in collaboration with Technical Committee ISO/TC 34 "Agricultural food
products".
According to the CEN/CENELEC Internal Regulations, the national standards organizations of
the following countries are bound to announce this CEN Technical Specification: Austria,
Belgium, 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.
TECHNICAL ISO/TS
SPECIFICATION 17764-1
First edition
2002-11-01
Animal feeding stuffs — Determination of
the content of fatty acids —
Part 1:
Preparation of methyl esters
Aliments des animaux — Détermination de la teneur en acides gras —
Partie 1: Préparation des esters méthyliques
Reference number
ISO/TS 17764-1:2002(E)
©
ISO 2002
ISO/TS 17764-1:2002(E)
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ISO/TS 17764-1:2002(E)
Foreword
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technical committee may decide to publish other types of normative document:
— an ISO Publicly Available Specification (ISO/PAS) represents an agreement between technical experts in
an ISO working group and is accepted for publication if it is approved by more than 50 % of the members
of the parent committee casting a vote;
— an ISO Technical Specification (ISO/TS) represents an agreement between the members of a technical
committee and is accepted for publication if it is approved by 2/3 of the members of the committee
casting a vote.
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further three years, revised to become an International Standard, or withdrawn. If the ISO/PAS or ISO/TS is
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ISO/TS 17764-1 was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 10,
Animal feeding stuffs.
ISO/TS 17764 consists of the following parts, under the general title Animal feeding stuffs — Determination of
the content of fatty acids:
Part 1: Preparation of methyl esters
Part 2: Gas chromatographic method
TECHNICAL SPECIFICATION ISO/TS 17764-1:2002(E)
Animal feeding stuffs — Determination of the content of fatty
acids —
Part 1:
Preparation of methyl esters
1 Scope
ISO/TS 17764 specifies methods for the quantitative determination of individual fatty acids and of the sum of
the fatty acids (elutable fatty acids).
This part of ISO/TS 17764 specifies two methods for preparing the methyl esters of fatty acids of animal and
vegetable fats, oils and fatty acid mixtures for raw materials for compound animal feeds, and fatty acids
originating from fat extracts of animal feeding stuffs, including fats and fatty acid mixtures containing butyric
acid.
The general method, the boron trifluoride (BF ) method, is concerned with the preparation of methyl esters of
fatty acids with six or more C atoms, originating from fats, oils and free fatty acids.
The KOH/HCl method is concerned with the preparation of methyl esters of fatty acids with four or more C
atoms. This method can also be used for the quantitative determination of fatty acids with a chain length
shorter than ten C atoms in free fatty acid mixtures.
The methyl esters produced can be used for gas-liquid chromatography (GLC).
NOTE 1 Unsaponifiable materials are not removed and can, when present in considerable amounts, interfere with the
chromatographic analysis.
NOTE 2 ISO/TS 17764-2 describes the application of gas chromatography with capillary columns and flame ionization
detection for the determination of the content of fatty acids in a fat by making use of the methyl esters of the fatty acids
obtained in accordance with the methods specified in this part of ISO/TS 17764.
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 661:1989, Animal and vegetable fats and oils Preparation of test sample
ISO 3696:1987, Water for analytical laboratory use Specification and test methods
ISO 6492:1999, Animal feeding stuffs Determination of fat content
ISO/TS 17764-1:2002(E)
3 Fat extraction
3.1 General
Extract the fat for determination of the content of the saponifiable fatty acids in an animal feeding stuff or
mixed feed in accordance with the category of the feeding stuff, as described in ISO 6492:1999, with the
following amendments.
3.2 Samples of category A
Perform a fat extraction in accordance with 9.5.1 of ISO 6492:1999.
Evaporate the solvent with a rotating evaporator in a water bath at a temperature of not more than 40 °C.
Then dry the residue for 2 h in a vacuum drying oven at 40 °C ± 2 °C.
3.3 Samples of category B
Extract the fat in two steps. For the first step, proceed in accordance with 9.5.1 of ISO 6492:1999, treating the
test portion as described in 9.3 of ISO 6492:1999 as a sample of category A.
Collect the fat extract in a dry flask. Allow the solvent to evaporate from the residue by exposing the thimble to
the air.
Perform a hydrolysis of the residue in accordance with 9.4 of ISO 6492:1999.
After hydrolysis, dry the residue in an extraction thimble for 60 min in a vacuum drying oven at 40 °C ± 2 °C.
Extract the residue according to 9.5.1 of ISO 6492:1999.
Add the fat extract to the first extract.
Evaporate the solvent with a rotating evaporator in a water bath at a temperature of not more than 40 °C and
dry the
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