SIST EN 14538:2025
(Main)Fat and oil derivatives - Fatty acid methyl ester (FAME) - Determination of Ca, K, Mg and Na content by optical emission spectral analysis with inductively coupled plasma (ICP OES)
Fat and oil derivatives - Fatty acid methyl ester (FAME) - Determination of Ca, K, Mg and Na content by optical emission spectral analysis with inductively coupled plasma (ICP OES)
This document specifies a procedure for the direct determination of the soap building elements Calcium (Ca), Magnesium (Mg), Sodium (Na) and Potassium (K) in fatty acid methyl esters (FAME) by ICP OES at levels of about 1 mg/kg to 10 mg/kg.
Erzeugnisse aus pflanzlichen und tierischen Fetten und Ölen - Fettsäure-Methylester (FAME) - Bestimmung des Ca-, K-, Mg- und Na-Gehaltes durch optische Emissionsspektralanalyse mit induktiv gekoppeltem Plasma (ICP OES)
Dieses Dokument legt ein Verfahren zur direkten Bestimmung des Gehalts der Seifenbildner Calcium (Ca), Magnesium (Mg), Natrium (Na), Kalium (K) sowie Phosphor (P) in Fettsäure-Methylester (FAME, en: fatty acid methyl esters) mittels ICP OES fest.
Die Massenanteile jeder Komponente oder der Kombinationen von Komponenten, für die dieses Verfahren anwendbar ist, sind in Tabelle 1 angegeben.
Tabelle 1 - Anwendungsbereiche für jedes Element
Element Anwendungsbereich
mg/kg
Ca 0,3 bis 5,4
Mg 0,3 bis 4,6
Na 0,4 bis 5,0
K 0,6 bis 5,3
P 1,0 bis 5,0
Ca + Mg 0,5 bis 9,4
Na + K 1,0 bis 9,9
Ca + Mg + Na + K 1,4 bis 19,3
WARNUNG - Die Anwendung dieses Dokuments kann die Anwendung gefährlicher Stoffe, Arbeitsgänge und Geräte mit sich bringen. Dieses Dokument beansprucht nicht, alle damit verbundenen Sicherheitsprobleme zu behandeln. Es liegt in der Verantwortung der Person, die das Dokument anwendet, vor der Anwendung geeignete Maßnahmen für die Sicherheit und den Gesundheitsschutz zu ergreifen, und die Geltung weiterer diesbezüglicher Auflagen zu prüfen.
ANMERKUNG Für die Zwecke dieses Dokuments wird zur Angabe des Volumenanteils φ einer Substanz der Ausdruck "% (V/V)" verwendet.
Produits dérivés des corps gras - Esters méthyliques d'acides gras (EMAG) - Détermination de la teneur en Ca, K, Mg et Na par spectrométrie d'émission optique avec plasma à couplage inductif (ICP OES)
Le présent document spécifie une méthode de dosage direct des teneurs en calcium (Ca), en magnésium (Mg), en sodium (Na) et en potassium (K), éléments susceptibles de former des savons, ainsi que de la teneur en phosphore (P) dans les esters méthyliques d'acides gras (EMAG) par ICP OES.
Les concentrations pour chaque composé ou combinaison de composés auxquelles cette méthode est applicable sont indiquées dans le Tableau 1.
Tableau 1 - Champs d’application pour chaque élément
Elément Champ d’application
mg/kg
Ca 0,3 - 5,4
Mg 0,3 - 4,6
Na 0,4 - 5,0
K 0,6 - 5,3
P 1,0 - 5,0
Ca + Mg 0,5 - 9,4
Na + K 1,0 - 9,9
Ca + Mg + Na + K 1,4 - 19,3
AVERTISSEMENT - L'utilisation du présent document peut impliquer des produits, des opérations et des équipements à caractère dangereux. Le présent document n'est pas censé aborder tous les problèmes de sécurité concernés par son usage. Il est de la responsabilité des utilisateurs de ce document de prendre les mesures appropriées pour assurer la sécurité et préserver la santé du personnel avant son application, et pour répondre aux exigences réglementaires et statutaires à cette fin.
NOTE Pour les besoins du présent document, l'expression "% (V/V)" est employée pour représenter la fraction volumique, φ, d’un matériau.
Derivati maščob in olj – Metil estri maščobnih kislin (FAME) – Določevanje Ca, K, Mg in Na z optično emisijsko spektometrijo z induktivno sklopljeno plazmo (ICP OES)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-marec-2025
Derivati maščob in olj – Metil estri maščobnih kislin (FAME) – Določevanje Ca, K,
Mg in Na z optično emisijsko spektometrijo z induktivno sklopljeno plazmo (ICP
OES)
Fat and oil derivatives - Fatty acid methyl ester (FAME) - Determination of Ca, K, Mg and
Na content by optical emission spectral analysis with inductively coupled plasma (ICP
OES)
Erzeugnisse aus pflanzlichen und tierischen Fetten und Ölen - Fettsäure-Methylester
(FAME) - Bestimmung des Ca-, K-, Mg- und Na-Gehaltes durch optische
Emissionsspektralanalyse mit induktiv gekoppeltem Plasma (ICP OES)
Produits dérivés des corps gras - Esters méthyliques d'acides gras (EMAG) -
Détermination de la teneur en Ca, K, Mg et Na par spectrométrie d'émission optique
avec plasma à couplage inductif (ICP OES)
Ta slovenski standard je istoveten z: EN 14538:2025
ICS:
71.040.40 Kemijska analiza Chemical analysis
75.160.20 Tekoča goriva Liquid fuels
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EN 14538
EUROPEAN STANDARD
NORME EUROPÉENNE
January 2025
EUROPÄISCHE NORM
ICS 67.200.10 Supersedes EN 14538:2006
English Version
Fat and oil derivatives - Fatty acid methyl ester (FAME) -
Determination of Ca, Mg, Na, K and P content by optical
emission spectral analysis with inductively coupled
plasma (ICP OES)
Produits dérivés des corps gras - Esters méthyliques Erzeugnisse aus pflanzlichen und tierischen Fetten und
d'acides gras (EMAG) - Détermination de la teneur en Ölen - Fettsäure-Methylester (FAME) - Bestimmung
Ca, Mg, Na, K et P par spectrométrie d'émission optique des Ca-, Mg-, Na-, K-, und P-Gehaltes durch optische
avec plasma à couplage inductif (ICP OES) Emissionsspektralanalyse mit induktiv gekoppeltem
Plasma (ICP OES)
This European Standard was approved by CEN on 25 November 2024.
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, Türkiye 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
© 2025 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 14538:2025 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 4
5 Reagents . 5
6 Apparatus . 5
7 Sampling . 6
8 Preparation of the calibration solutions and the blank solution . 6
8.1 General . 6
8.2 Calibration solutions . 7
8.3 Calibration check solution . 7
9 Calibration . 7
9.1 General . 7
9.2 Calibration . 8
9.3 Check of calibration . 8
10 Sample analysis . 8
10.1 Sample preparation . 8
10.2 Sample preparation of high concentration samples . 8
10.3 Measurement . 8
11 Calculation . 9
12 Expression of results . 9
13 Precision . 9
13.1 General . 9
13.2 Repeatability, r . 9
13.3 Reproducibility, R . 9
14 Test report . 10
Bibliography . 11
European foreword
This document (EN 14538:2025) has been prepared by Technical Committee CEN/TC 19 “Gaseous and
liquid fuels, lubricants and related products of petroleum, synthetic and biological origin”, 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 July 2025, and conflicting national standards shall be
withdrawn at the latest by July 2025.
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 will supersede EN 14538:2006.
— update of the precision details for Ca, Mg, Na and K following the statistical analysis of new
interlaboratory tests data [1] in accordance with EN ISO 4259-1 [2];
— inclusion of the determination of P content with precision details obtained from the statistical
analysis of new interlaboratory tests data [1] in accordance with EN ISO 4259-1 [2];
— addition of Clause 3 “Terms and definitions” and renumbering of the other clauses accordingly;
— addition of a Bibliography section with two references.
Any feedback and questions on this document should be directed to the users’ national standards body.
A complete listing of these bodies can be found on the CEN website.
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, Türkiye and the United
Kingdom.
1 Scope
This document specifies a procedure for the direct determination of the content of the soap building
elements Calcium (Ca), Magnesium (Mg), Sodium (Na) and Potassium (K) as well as Phosphorus (P) in
fatty acid methyl esters (FAME) by ICP OES.
The concentrations of each component or the combinations of some to which this method is applicable
are given in Table 1.
Table 1 — Scope ranges for each element
Element Scope range
mg/kg
Ca 0,3 – 5,4
Mg 0,3 – 4,6
Na 0,4 – 5,0
K 0,6 – 5,3
P 1,0 – 5,0
Ca + Mg 0,5 – 9,4
Na + K 1,0 – 9,9
Ca + Mg + Na + K 1,4 – 19,3
WARNING — The use of this document can involve hazardous materials, operations and equipment. This
document does not purport to address all of the safety problems associated with its use. It is the
responsibility of the user of this document to establish appropriate safety and health practices and
determine the applicability of regulatory limitations prior to use.
NOTE For the purposes of this document, the term “% (V/V)” is used to represent the volume fraction, φ, of a
material.
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)
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https://www.iso.org/obp/
— IEC Electropedia: available at https://www.electropedia.org/
4 Principle
An exactly weighed amount of FAME sample is diluted minimum 1 + 1 with kerosene. This solution is
introduced directly into the plasma of an ICP OES spectrometer. The analyte content is determined by
comparison with calibration solutions. The contents of Calcium, Magnesium, Sodium, Potassium and
Phosphorus are reported.
NOTE 1 An internal standard can be used to correct viscosity effects.
NOTE 2 All examples in this document are calculated for a dilution of the samples of 1 + 2 with kerosene.
5 Reagents
5.1 “Distilled” FAME not containing any of the elements to be analyzed, as indicated by the absence of
any peak at the different reference wavelengths (see Table 2).
5.2 Kerosene, boiling range included between 145 °C and 250 °C, containing less than 0,05 mg/kg of
analyte elements (check if you can see any peak).
NOTE In case of unstable plasma or in case of special laboratory requirements, kerosene can be substituted by
other suitable solvents, provided that they are free of analytes.
5.3 Element standard solutions (Ca, Mg, Na, K, P), dissolved in oil, e.g. 1 000 mg/kg per element.
These are available as single element or multi element standard solutions.
5.4 Calcium, Magnesium, Sodium, Potassium, Phosphorus intermediate working standard
(20 mg/kg).
Accurately weigh about 0,4 g to the nearest 0,1 g of each element standard solution (5.3) into a 50 ml
bottle (6.1). Add distilled FAME (5.1) to a total mass of about 20,0 g to the nearest 0,1 g. Calculate the
exact concentrations for the intermediate working standard, taking into account the exact weights.
NOTE Some commercial multi element standard solutions are available on the market.
5.5 Argon, with minimum purity w (Ar) = 99,996 % (V/V).
Small amounts of oxygen may be added to the argon gas stream (30 ml/min to 100 ml/min) to prevent
carbon deposits in the area of the plasma torch.
NOTE When adding oxygen, it is important to note that the sensitivity in the UV is greatly reduced (e.g.
P 177nm). With some instruments it can therefore be necessary to analyse the samples once with (for Na and K)
and once without oxygen addition (for P).
6 Apparatus
Commercial laboratory and glass equipment, in conjunction with the following:
6.1 30 ml or 50 ml bottles with cap, preferably made of PP, LDPE, HDPE or Polytetrafluoroethylene
(PTFE) FEP or PFA.
To avoid phosphorus pollution due to the phosphates contained in the detergents used for washing the
bottles, rinse the latter at least twice with an approximate 5 mol/l solution of hydrochloric acid. Then
rinse with dist
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