prEN 16997

SLOVENSKI STANDARD
01-julij-2024
Tekoči naftni proizvodi - Določanje žvepla v motornem gorivu etanol (E85) -
Metoda z valovno disperzivno rentgensko fluorescenčno spektrometrijo
Liquid petroleum products - Determination of the sulfur content in Ethanol (E85)
automotive fuel- Wavelength dispersive X-ray fluorescence spectrometric method
Flüssige Mineralölerzeugnisse - Bestimmung des Schwefelgehalts in Ethanolkraftstoff
(E85) - Wellenlängendispersives Röntgenfluoreszenz-Spektrometrie-Verfahren
Produits pétroliers liquides - Détermination de la teneur en soufre dans le carburant
éthanol pour automobiles (E85) - Méthode spectrométrique par fluorescence de rayons
X dispersive en longueur d'onde
Ta slovenski standard je istoveten z: prEN 16997
ICS:
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
75.160.20 Tekoča goriva Liquid fuels
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

DRAFT
EUROPEAN STANDARD
NORME EUROPÉENNE
EUROPÄISCHE NORM
July 2024
ICS 75.160.20 Will supersede EN 16997:2017
English Version
Liquid petroleum products - Determination of the sulfur
content in Ethanol (E85) automotive fuel- Wavelength
dispersive X-ray fluorescence spectrometric method
Produits pétroliers liquides - Détermination de la Flüssige Mineralölerzeugnisse - Bestimmung des
teneur en soufre dans des carburant automobile Schwefelgehalts in Ethanolkraftstoff (E85) -
Ethanol (E85) - Méthode de fluorescence de rayons X Wellenlängendispersives Röntgenfluoreszenz-
dispersive en longuer d'onde Spektrometrie-Verfahren
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 16997:2024 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 and materials . 4
6 Apparatus . 5
7 Sampling . 5
8 Preparation of calibration solutions . 6
8.1 Interferences . 6
8.1.1 Background . 6
8.1.2 FP method . 7
8.1.3 Correction table . 7
8.2 Blank calibration solution . 7
8.3 Stock solution . 7
8.4 Calibration solutions . 7
8.5 Storage and stability of the calibration solutions . 7
9 Settings . 8
9.1 Measuring parameters . 8
9.2 Optimization . 8
9.2.1 Monochromatic excitation . 8
9.2.2 Polychromatic excitation . 8
9.3 Performance check of the spectrometer . 8
10 Calibration . 8
10.1 General . 8
10.2 Calibration solutions . 8
10.3 Calibration curves . 9
10.3.1 Calibration without matrix correction . 9
10.3.2 Calibration with matrix correction . 9
10.4 Checking . 10
11 Procedure. 10
12 Expression of results . 11
13 Precision . 11
13.1 General . 11
13.2 Repeatability . 11
13.3 Reproducibility . 11
14 Test report . 12
Annex A (informative) Fundamental parameters method background . 13
Bibliography . 14

European foreword
This document (prEN 16997:2024) 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 16997:2017.
This second edition includes the following significant changes compared with the previous edition
EN 16997:2017:
— addition of Clause 3 “Terms and definitions” and renumbering of the other clauses accordingly;
— correction of Formula (3) in 10.3.1.
The methodology described in this document is based on EN ISO 20884 [1] and EN 15485 [2].

1 Scope
This document specifies a wavelength-dispersive X-ray fluorescence (WDXRF) test method for the
determination of the sulfur content in ethanol (E85) automotive fuel [3], containing ethanol between
50 % (V/V) and 85 % (V/V), from 5 mg/kg to 20 mg/kg, using instruments with either monochromatic
or polychromatic excitation.
NOTE 1 Sulfur contents higher than 20 mg/kg can be determined after sample dilution with an appropriate
solvent. However, the precision was not established for diluted samples.
NOTE 2 For the purposes of this document, the terms “% (m/m)” and “% (V/V)” are used to represent the mass
fraction (µ) and the volume fraction (φ) of a material respectively.
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.
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)
EN ISO 22854, Liquid petroleum products — Determination of hydrocarbon types and oxygenates in
automotive-motor gasoline and in ethanol (E85) automotive fuel — Multidimensional gas chromatography
method (ISO 22854)
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:
— IEC Electropedia: available at https://www.electropedia.org/
— ISO Online browsing platform: available at https://www.iso.org/obp/ui
4 Principle
The sample under analysis is exposed in a sample cell to the primary radiation of an X-ray tube. The count
rates of the S K-L X-ray fluorescence and the count rate of the background radiation are measured.
2,3
The correlation between the pulse rate and the concentration is calculated by software. The matrix effects
are compensated either on the basis of fundamental parameters or using a correction table. The sulfur
content is then determined using this calibration.
5 Reagents and materials
5.1 General
Compounds with a minimum purity of 99 % (m/m) as in 5.2 to 5.4. Where the purity of these compounds
is less than 99 % (m/m), the concentrations and nature of all impurities shall be established.
A correction for chemical impurity may be applied when the sulfur content is known with accuracy.
Certified reference materials (CRMs) from accredited suppliers are suitable alternatives to the
compounds listed in 5.2 to 5.4.
5.2 Dibutylsulfide, of nominal sulfur content 21,92 % (m/m), or dibutyldisulfide, of nominal sulfur
content 35,95 % (m/m), used as a calibrating substance for sulfur.
5.3 Ethanol absolute, of a purity not less than 99 %, for use as a compound of the blank solution (8.2),
high purity grade, with a sulfur content < 1 mg/kg.
Check the blank solution (8.2) prior to use with the spectrometer (6.2). A signal for sulfur shall not be
detectable.
5.4 n-Heptane, of a purity not less than 99 %, for use as a compound of the blank solution (8.2), high
purity grade, with a sulfur content < 1 mg/kg.
Check the blank solution (8.2) prior to use with the spectrometer (6.2). A signal for sulfur shall not be
detectable.
6 Apparatus
6.1 Software to set up a calibration and for the appli
...