kSIST FprEN 14538:2024

SLOVENSKI STANDARD
oSIST prEN 14538:2024
01-februar-2024
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: prEN 14538
ICS:
75.160.20 Tekoča goriva Liquid fuels
oSIST prEN 14538:2024 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

oSIST prEN 14538:2024
oSIST prEN 14538:2024
DRAFT
EUROPEAN STANDARD
prEN 14538
NORME EUROPÉENNE
EUROPÄISCHE NORM
February 2024
ICS 75.160.20 Will supersede 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, K, Mg et Na par spectrométrie d'émission optique des Ca-, K-, Mg- und Na-Gehaltes durch optische
avec plasma à couplage inductif (ICP OES) Emissionsspektralanalyse mit induktiv gekoppeltem
Plasma (ICP OES)
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee
CEN/TC 19.
If this draft becomes a European Standard, 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.

This draft European Standard was established by CEN 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.
Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are
aware and to provide supporting documentation.

Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without
notice and shall not be referred to as a European Standard.

EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2024 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 14538:2024 E
worldwide for CEN national Members.

oSIST prEN 14538:2024
prEN 14538:2024 (E)
Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 5
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
oSIST prEN 14538:2024
prEN 14538:2024 (E)
European foreword
This document (prEN 14538:2024) 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 document is currently submitted to the CEN Enquiry.
This document will supersede EN 14538:2006.
prEN 14538:2024 includes the following significant technical changes with respect to 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.
oSIST prEN 14538:2024
prEN 14538:2024 (E)
1 Scope
This document specifies a procedure for the direct determination 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 0,31 – 5,44
Mg 0,31 – 4,57
Na 0,43 – 4,98
K 0,59 – 5,34
P 0,97 – 5,00
Ca + Mg 0,53 – 9,40
Na + K 1,05 – 9,94
Ca + Mg + Na + K 1,42 – 19,35
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/
oSIST prEN 14538:2024
prEN 14538:2024 (E)
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, containing less than 0,05 mg/kg of analyte elements (check if you can see any peak).
NOTE Some commercial blank FAME with certificate are available on the market.
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 older instruments it may 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 distilled water and dry. To avoid contamination of the test samples, all solutions should be
prepared in plastic bottles. Surfaces which can come in contact with the solutions should not be touched
by hand.
6.2 Analytical balance, capable of displaying to the nearest 0,1 mg.
oSIST prEN 14538:2024
prEN 14538:2024 (E)
6.3 ICP OES spectrometer
6.3.1 General
Simultaneous and equally suitable sequential spectrometer ICP OES spectrometer equipped for the
analysis of organic liquids, with a high-frequency generator with 27 MHz or 40 MHz and a nebuliser
suitable for organic solvents. The use of a feed pump for sample introduction into the nebuliser is
required. Pump tubing shall be suitable for organic use. Both setup and operation of the ICP OES
spectrometer shall be done in accordance with operating instructions of the manufacturer.
The use of an ICP OES with a vertical torch and a radial view (or a dual radial view) is advisable to avoid
car
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