Fat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of oxidation stability (accelerated oxidation test)

This European Standard specifies a method for the determination of the oxidation stability of fatty acid methyl esters (FAME) at 110 °C, by means of measuring the induction period up to 48 h.
NOTE 1   EN 15751 [1] describes a similar test method for oxidation stability determination of pure fatty acid methyl esters and of blends of FAME with petroleum-based diesel containing 2 % (V/V) of FAME at minimum.
NOTE 2   The precision statement of this test method was determined in a Round Robin exercise with induction periods up to 8,5 h, thus covering the limit value in EN 14214. Results from precision studies on EN 15751 indicate that the precision statement is valid for induction periods up to 48 h but not for higher values.
NOTE 3   Limited studies on EN 15751 with EHN (2-ethyl hexyl nitrate) on FAME blends indicated that the stability is reduced to an extent which is within the reproducibility of the test method. It is likely that the oxidation stability of pure FAMEs is also reduced in the presence of EHN when EN 14112 is used for testing.

Erzeugnisse aus pflanzlichen und tierischen Fetten und Ölen - Fettsäure-Methylester (FAME) - Bestimmung der Oxidationsstabilität (beschleunigte Oxidationsprüfung)

Dieses Dokument legt ein Verfahren zur Bestimmung der Oxidationsstabilität von Fettsäure-Methylestern (FAME) bei 110 °C mittels Messung der Induktionszeit bis zu 48 h fest.
Bei längeren Induktionszeiten als 8,5 h ist die Präzision nicht durch die Präzisionsangabe dieses Verfahren abgedeckt.
ANMERKUNG 1 EN 15751 [1] beschreibt ein ähnliches Prüfverfahren zur Bestimmung der Oxidationsstabilität von reinen Fettsäure-Methylestern und von Mischungen von FAME mit aus Erdöl hergestellten Dieselkraftstoffen, die mindestens 2 % (V/V) FAME enthalten.
ANMERKUNG 2 Die Präzisionsangabe dieses Prüfverfahrens wurde in einem Ringversuch mit Induktionszeiten bis zu 8,5 h bestimmt und deckt damit den Grenzwert in EN 14214 ab. Die Ergebnisse aus Untersuchungen zur Präzision der EN 15751 zeigten, dass die angegebene Präzision für Induktionszeiten bis zu 48 h, nicht jedoch für höhere Werte, gültig ist.
ANMERKUNG 3 Begrenzte Studien zur EN 15751 mit EHN (2-Ethylhexylnitrat) mit FAME-Mischungen wiesen darauf hin, dass sich die Stabilität in einem Umfang verringert, der innerhalb der Vergleichbarkeit dieses Prüfverfahrens liegt. Es ist wahrscheinlich, dass die Oxidationsstabilität von reinen Fettsäure-Methylestern in Gegenwart von EHN ebenfalls verringert wird, wenn die EN 14112 zur Prüfung angewendet wird.
ANMERKUNG 4 Für die Zwecke dieser Europäischen Norm wird zur Angabe des Volumenanteils einer Substanz der Ausdruck „% (V/V)“ verwendet.

Produits dérivés des corps gras - Esters méthyliques d'acides gras (EMAG) - Détermination de la stabilité à l'oxydation (Essai d'oxydation accélérée)

Le présent document spécifie une méthode de détermination de la stabilité à l’oxydation des esters méthyliques d'acides gras (EMAG) à 110 °C, en mesurant la période d'induction pendant une durée pouvant atteindre 48 h.
Pour les périodes d'induction supérieures à 8,5 h, la fidélité n’est pas couverte par les données de fidélité de la présente méthode.
NOTE 1 L’EN 15751 [1] décrit une méthode d’essai similaire permettant de déterminer la stabilité à l’oxydation des esters méthyliques d’acides gras et des mélanges d’EMAG avec un carburant à base de pétrole contenant au moins 2 % (V/V) d’EMAG.
NOTE 2 Les données de fidélité de la présente méthode ont été déterminées lors d'un essai interlaboratoires avec des périodes d’induction pouvant atteindre 8,5 h, couvrant ainsi la valeur limite indiquée dans l’EN 14214. Les résultats des études de fidélité sur l’EN 15751 indiquent que les données de fidélité sont valables pour des périodes d’induction pouvant atteindre 48 h au maximum.
NOTE 3 Des études limitées sur l’EN 15751 avec l’EHN (2-éthylhexyl nitrate) sur les mélanges d’EMAG ont indiqué que la stabilité est réduite dans les limites de reproductibilité de la méthode d’essai. Il semblerait que la stabilité à l’oxydation des EMAG purs soit également réduite en présence d’EHN lorsque l’EN 14112 est utilisée pour les essais.
NOTE 4 Pour les besoins du présent document, le terme « % (V/V) » est utilisé pour représenter la fraction volumique.

Derivati maščob in olj - Metilni estri maščobnih kislin (FAME) - Določevanje oksidativne stabilnosti (metoda s pospešeno oksidacijo)

General Information

Status
Published
Public Enquiry End Date
19-Feb-2020
Publication Date
10-Dec-2020
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
08-Dec-2020
Due Date
12-Feb-2021
Completion Date
11-Dec-2020

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SLOVENSKI STANDARD
SIST EN 14112:2021
01-januar-2021
Nadomešča:
SIST EN 14112:2016
Derivati maščob in olj - Metilni estri maščobnih kislin (FAME) - Določevanje
oksidativne stabilnosti (metoda s pospešeno oksidacijo)

Fat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of oxidation

stability (accelerated oxidation test)

Erzeugnisse aus pflanzlichen und tierischen Fetten und Ölen - Fettsäure-Methylester

(FAME) - Bestimmung der Oxidationsstabilität (beschleunigte Oxidationsprüfung)
Produits dérivés des corps gras - Esters méthyliques d'acides gras (EMAG) -
Détermination de la stabilité à l'oxydation (Essai d'oxydation accélérée)
Ta slovenski standard je istoveten z: EN 14112:2020
ICS:
67.200.10 Rastlinske in živalske Animal and vegetable fats
maščobe in olja and oils
SIST EN 14112:2021 en,fr,de

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

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SIST EN 14112:2021
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SIST EN 14112:2021
EN 14112
EUROPEAN STANDARD
NORME EUROPÉENNE
November 2020
EUROPÄISCHE NORM
ICS 67.200.10 Supersedes EN 14112:2016
English Version
Fat and oil derivatives - Fatty Acid Methyl Esters (FAME) -
Determination of oxidation stability (accelerated oxidation
test)

Produits dérivés des corps gras - Esters méthyliques Erzeugnisse aus pflanzlichen und tierischen Fetten und

d'acides gras (EMAG) - Détermination de la stabilité à Ölen - Fettsäure-Methylester (FAME) - Bestimmung

l'oxydation (Essai d'oxydation accélérée) der Oxidationsstabilität (beschleunigte

Oxidationsprüfung)
This European Standard was approved by CEN on 25 October 2020.

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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,

Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and

United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 14112:2020 E

worldwide for CEN national Members.
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SIST EN 14112:2021
EN 14112:2020 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

1 Scope .................................................................................................................................................................... 4

2 Normative references .................................................................................................................................... 4

3 Terms and definitions ................................................................................................................................... 4

4 Principle ............................................................................................................................................................. 5

5 Chemicals ........................................................................................................................................................... 5

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

7 Sampling ............................................................................................................................................................. 7

8 Preparation of measurement ..................................................................................................................... 8

8.1 Preparation of test sample .......................................................................................................................... 8

8.2 Preparation of apparatus ............................................................................................................................. 8

8.2.1 Cleaning procedure ........................................................................................................................................ 8

8.2.2 Temperature correction ............................................................................................................................... 8

9 Measurement .................................................................................................................................................... 9

10 Calculation and Evaluation ....................................................................................................................... 12

10.1 Automatic evaluation .................................................................................................................................. 12

10.2 Manual evaluation ....................................................................................................................................... 14

11 Expression of results ................................................................................................................................... 15

12 Precision .......................................................................................................................................................... 15

12.1 General ............................................................................................................................................................. 15

12.2 Repeatability, r .............................................................................................................................................. 15

12.3 Reproducibility, R ........................................................................................................................................ 15

13 Test report ...................................................................................................................................................... 15

Annex A (informative) Background of the method ......................................................................................... 16

Annex B (informative) Results of an Interlaboratory Study ........................................................................ 17

Bibliography ................................................................................................................................................................. 18

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SIST EN 14112:2021
EN 14112:2020 (E)
European foreword

This document (EN 14112:2020) has been prepared by Technical Committee CEN/TC 307 “Oilseeds, vegetable

and animal fats and oils and their by-products - Methods of sampling and analysis”, the secretariat of which is

held by AFNOR.

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 May 2021, and conflicting national standards shall be withdrawn at the

latest by May 2021.

Attention is drawn to the possibility that some of the elements of this document may be the subject of patent

rights. CEN shall not be held responsible for identifying any or all such patent rights.

This document supersedes EN 14112:2016.
Significant changes between this document and EN 14112:2016 are:
— change of Figure 2, removal of dimension between air inlet and heating block;
— introduction removed;
— document revised editorially.

According to the CEN-CENELEC Internal Regulations, the national standards organisations of the following

countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech

Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia,

Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of North Macedonia, Romania,

Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.

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SIST EN 14112:2021
EN 14112:2020 (E)
1 Scope

This document specifies a method for the determination of the oxidation stability of fatty acid methyl esters

(FAME) at 110 °C, by means of measuring the induction period up to 48 h.

For induction periods higher than 8,5 h the precision is not covered by the precision statement of this method.

NOTE 1 EN 15751 [1] describes a similar test method for oxidation stability determination of pure fatty acid methyl

esters and of blends of FAME with petroleum-based diesel containing 2 % (V/V) of FAME at minimum.

NOTE 2 Limited studies on EN 15751 with EHN (2-ethyl hexyl nitrate) on FAME blends indicated that the stability is

reduced to an extent which is within the reproducibility of the test method. It is likely that the oxidation stability of pure

FAMEs is also reduced in the presence of EHN when EN 14112 is used for testing.

NOTE 3 For the purposes of this document, the term “% (V/V)” is used to represent the volume fraction.

2 Normative references

The following documents are referred to in the text in such a way that some or all of their content constitutes

requirements 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.
EN ISO 3170, Petroleum liquids - Manual sampling (ISO 3170)
EN ISO 3171, Petroleum liquids - Automatic pipeline sampling (ISO 3171)
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

• IEC Electropedia: available at http://www.electropedia.org/
• ISO Online browsing platform: available at https://www.iso.org/obp
3.1
induction period

time which passes between the moment when the measurement is started and the moment when the formation

of oxidation products begins to increase rapidly
3.2
oxidation stability

induction period determined according to the procedure specified in this document, expressed in hours

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SIST EN 14112:2021
EN 14112:2020 (E)
4 Principle

A stream of purified (dried) air is passed through the sample which has been heated to the target temperature

which is 110 °C in the usual application of the method. Volatile compounds are formed during the oxidation

process. They are passed, together with the air, into a flask containing demineralized or distilled water, and

equipped with a conductivity electrode. The electrode is connected to a measuring and recording device. It

indicates the end of the induction period by rapid increase of the conductivity due to the dissociation of volatile

carboxylic acids produced during the oxidation process and absorbed in the water. For more details on the

background of the method see Annex A.
5 Chemicals
Use only chemicals of analytical grade and distilled or demineralized water.

5.1 Ternary solvent mixture, consisting of methanol/toluene/acetone 1:1:1 (by volume).

5.2 Alkaline laboratory glass cleaning solution.
5.3 2-Propanol.
6 Apparatus
Usual laboratory equipment and glassware, together with the following:

6.1 Device for the determination of oxidation stability, comprising the following parts (see Figures 1

and 2) .

6.1.1 Air filter, comprising a tube fitted with filter paper at the ends and filled with a molecular sieve (6.6),

connected to the suction end of a pump.
6.1.2 Gas membrane pump, with an adjustable flow rate of (10 ± 1,0) l/h.

6.1.3 Reaction vessels of borosilicate glass, provided with a sealing cap. The sealing cap shall be fitted with a

gas inlet and outlet tube.

6.1.4 Closed measurement cells, of approximately 150 ml capacity, with an air inlet tube extending to the

bottom inside of the vessel. The cell shall have ventilation holes at the top.

6.1.5 Electrodes, for measuring conductivity within a range of 0 μS/cm to 300 μS/cm aligned with the

dimensions of the measurement cell (6.1.4).
6.1.6 Measuring and recording apparatus, comprising:
a) an amplifier; and
b) a recorder registering the signal of each of the electrodes (6.1.5).

1) Rancimat is the trade name of a product supplied by Metrohm AG, Herisau, Switzerland; OSI is the trade name of a product supplied

by Omnion Inc., Rockland, Massachusetts, USA. This information is given for the convenience of users of this document and does not

constitute an endorsement by CEN or CENELEC of the products named. Equivalent products may be used if they can be shown to lead to

the same results.
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SIST EN 14112:2021
EN 14112:2020 (E)

6.1.7 Contact thermometer graduated in 0,1 °C or Pt 100 element to measure the block temperature, with

attachments for relay connection and an adjustable heating element; temperature scale 0 °C to 150 °C.

6.1.8 Heating source, 6.1.8.1 or 6.1.8.2

6.1.8.1 Heating block, made of cast aluminium, adjustable to a temperature up to (150 ± 0,1) °C. The block

shall be provided with holes for the reaction vessels (6.1.3) and an aperture for the contact thermometer

(6.1.7).

6.1.8.2 Heating bath, filled with oil suitable for temperatures up to 150 °C, and adjustable to the

nearest 0,1 °C.

6.2 Certified and calibrated thermometer or Pt100 element, with a temperature range up to 150 °C,

graduated in 0,1 °C.
Key
1 air filter (6.1.1) 5 electrode (6.1.5)

2 gas membrane pump with flow rate control (6.1.2) 6 measuring and recording apparatus (6.1.6)

3 reaction vessel (6.1.3) 7 contact thermometer or Pt 100 element (6.1.7)
4 measurement cell (6.1.4) 8 heating block (6.1.8.1)
Figure 1 — Schematic overview of apparatus
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SIST EN 14112:2021
EN 14112:2020 (E)
Key
1 measurement cell (6.1.4) 5 sample
2 electrode (6.1.5) 6 heating block (6.1.8.1)
3 distilled/demineralized water 7 air inlet
4 reaction vessel (6.1.3)

Figure 2 — Diagrammatic representation of heating block, reaction vessel and measurement cell

6.3 Measuring pipettes and/or measuring cylinders.
6.4 Oven, adjustable to a temperature up to (150 ± 3) °C.

6.5 Connecting hoses, flexible and made of inert material [polytetrafluoroethylene (PTFE) or silicone].

6.6 Molecular sieve, with moisture indicator, pore size 0,3 nm, dried in an oven set at 150 °C and cooled

down to room temperature in a desiccator before use.
6.7 Balance, capable of weighing with an accuracy of ± 0,1 g or less.
7 Sampling

Unless otherwise specified, sampling shall be conducted according to EN ISO 3170 or EN ISO 3171 and/or

should be in accordance with the requirements of national standards or regulations for the sampling.

It is important that the laboratory receives a sample which is truly representative and has not been damaged or

changed during tran
...

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