FprEN 18051
(Main)Automotive fuels - Determination of content of butoxy-benzene in middle distillates - Gas chromatographic method using a flame ionization detector (GC-FID)
Automotive fuels - Determination of content of butoxy-benzene in middle distillates - Gas chromatographic method using a flame ionization detector (GC-FID)
This document specifies a test method for the determination of the content of n-butyl phenyl ether (BPE, also known as butoxy-benzene) in gas oils, kerosene, diesel fuel and biodiesel blends. The method uses a two-column gas chromatograph with an FID-type of detector. The application range is 0,1 mg/l to 21,25 mg/l of BPE, with a limit of detection of 0,05 mg/l.
NOTE This corresponds to 1 % to 150 % of the average marking level of the ACCUTRACE™ Plus required by Commission Implementing Decision (EU) 2022/197 [1] of 17 January 2022 establishing a common fiscal marker for gas oils and kerosene.
The method is found to be applicable to determinations beyond this range or for specific other chemical markers that fall within the distillation temperature range of middle-distillates, but for that no precision has been determined.
WARNING —The use of this document may 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 to determine the applicability of regulatory limitations prior to use.
Mineralölerzeugnisse - Bestimmung von Gehalt von Butoxybenzol in Mitteldestillaten - Gaschromatographisches Verfahren mit Flammenionisationsdetektor (GC-FID)
Dieses Dokument legt ein Prüfverfahren für die Bestimmung des Gehalts an n-Butylphenylether (BPE, auch bekannt als Butoxybenzol) in Gasölen, Kerosin, Dieselkraftstoff und Biodieselmischungen fest. Bei dem Verfahren wird ein Zweisäulen-Gaschromatograph mit einem FID-Detektor verwendet. Der Anwendungsbereich reicht von 0,1 mg/l bis 21,25 mg/l BPE, mit einer Nachweisgrenze von 0,05 mg/l.
ANMERKUNG Das entspricht 1 % bis 150 % des vom Durchführungsbeschluss (EU) 2022/197 der Kommission [1] vom 17. Januar 2022 zur Bestimmung eines gemeinsamen Stoffes zur steuerlichen Kennzeichnung von Gasölen und Kerosin geforderten mittleren Gehalts an dem Kennzeichnungsstoff ACCUTRACETM PLUS.
Das Verfahren hat sich als anwendbar für Bestimmungen erwiesen, die über diesen Bereich hinausgehen, oder für bestimmte andere chemische Marker, die in den Destillationstemperaturbereich von Mitteldestillaten fallen, für die jedoch keine Präzision ermittelt wurde.
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 einschränkender Vorschriften zu ermitteln.
Carburants automobiles - Détermination de la teneur en butoxybenzène dans les distillats moyens - Méthode par chromatographie en phase gazeuse utilisant un détecteur à ionisation de flamme
Le présent document spécifie une méthode d'essai pour la détermination de la teneur en éther de n-butyl phényl (BPE, également connu sous le nom de butoxybenzène) dans les gazoles, le pétrole lampant, le carburant diesel et les mélanges de biodiesel. La méthode utilise un chromatographe en phase gazeuse à deux colonnes avec un détecteur de type DIF. Le domaine d'application est compris entre 0,1 mg/l et 21,25 mg/l de BPE, avec une limite de détection de 0,05 mg/l.
NOTE Cela correspond à une plage de 1 % à 150 % du niveau de marquage moyen de l'ACCUTRACE™ PLUS requis par la décision d'exécution (UE) 2022/197[1] de la Commission du 17 janvier 2022 établissant un marqueur fiscal commun pour les gazoles et le pétrole lampant.
La méthode s'avère applicable aux déterminations au-delà de cette fourchette ou pour d'autres marqueurs chimiques spécifiques qui se situent dans la fourchette de température de distillation des distillats moyens, mais pour lesquels aucune précision n'a été déterminée.
AVERTISSEMENT — L'utilisation du présent document peut impliquer la mise en œuvre de matériaux, d’opérations et de matériels dangereux. Le présent document ne prétend pas aborder tous les problèmes de sécurité associés à son utilisation. Il est de la responsabilité de l'utilisateur du présent document de prendre les mesures appropriées pour assurer la sécurité et préserver la santé du personnel avant l'application du présent document, et satisfaire aux exigences légales et réglementaires applicables à cet effet.
Motorna goriva - Določanje vsebnosti butoksibenzena v srednjih destilatih - Metoda plinske kromatografije z uporabo plamensko ionizacijskega detektorja (GC-FID)
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
01-december-2023
Motorna goriva - Določanje vsebnosti butoksibenzena v srednjih destilatih -
Metoda plinske kromatografije z uporabo plamensko ionizacijskega detektorja
(GC-FID)
Automotive fuels - Determination of content of butoxy-benzene in middle distillates - Gas
chromatographic method using a flame ionization detector (GC-FID)
Mineralölerzeugnisse - Bestimmung von Gehalt von Butoxybenzene in Mitteldestillaten –
Gaschromatographisches Verfahren mit Flammenionisationsdetektor
Produits pétroliers - Détermination de la teneur de butoxybenzene dans les distillats
moyens - Méthode par chromatographie gazeuse avec détecteur d'ionisation de flamme
Ta slovenski standard je istoveten z: prEN 18051
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
prEN 18051
NORME EUROPÉENNE
EUROPÄISCHE NORM
December 2023
ICS 75.160.40; 75.160.20
English Version
Automotive fuels - Determination of content of butoxy-
benzene in middle distillates - Gas chromatographic
method using a flame ionization detector (GC-FID)
Produits pétroliers - Détermination de la teneur de Mineralölerzeugnisse - Bestimmung von Gehalt von
butoxybenzene dans les distillats moyens - Méthode Butoxybenzene in Mitteldestillaten -
par chromatographie gazeuse avec détecteur Gaschromatographisches Verfahren mit
d'ionisation de flamme Flammenionisationsdetektor
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
© 2023 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 18051:2023 E
worldwide for CEN national Members.
prEN 18051:2023 (E)
Contents Page
European foreword . 3
Introduction . 4
1 Scope . 5
2 Normative references . 5
3 Terms, definitions and abbreviations . 5
3.1 Definitions . 5
3.2 Abbreviations . 5
4 Principle . 6
5 Reagents and materials . 6
6 Apparatus . 6
7 Sampling . 8
8 Preparation and handling of working solutions . 8
8.1 Preparation of stock calibration solution . 8
8.2 Preparation of working calibration solution (WCS) . 8
8.3 Preparation of linearity working solution (LWS) . 8
8.4 Storage of working solutions . 9
9 Apparatus preparation . 9
9.1 Gas chromatograph preparation . 9
9.2 System performance check . 9
9.2.1 Determine heart-cutting time . 9
9.2.2 Peak skew check. 9
9.2.3 Determine response factor . 10
10 Procedure . 10
10.1 Initial step . 10
10.2 Linearity check . 10
10.3 Validation analysis . 11
10.4 Sample analysis . 11
11 Calculation . 11
12 Expression of results . 12
13 Precision . 12
13.1 General. 12
13.2 Repeatability . 12
13.3 Reproducibility . 12
14 Test report . 12
Annex A (normative) Typical GC settings . 13
Bibliography . 15
prEN 18051:2023 (E)
European foreword
This document (prEN 18051:2023) 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 supports implementation in the market of the Decision [1] of the European Commission
with regards to common distillate fuel marking.
This document is currently submitted to the CEN Enquiry.
prEN 18051:2023 (E)
Introduction
For the proper functioning of the internal market, the European Commission has established Directives
providing for a common marking system to identify gas oils and kerosene, which have been released for
consumption exempt from excise duty, or which are subject to a reduced excise duty rate. In a review in
2019, the Commission’s evaluation identified the shortcomings of the actual marker (Solvent Yellow 124)
in terms of its lack of resilience to common removal methods.
Consequently, a new, colourless chemical marker, Butoxybenzene (CAS Registry Number 1126-79-0),
was chosen to replace Solvent Yellow 124 as of 18 January 2024. This product is commercially available
TM
as ACCUTRACE PLUS from DOW.
At the time of publication of the decision [1], a gas chromatography technique using a mass spectrometer
(GC-MS) as detector was promoted by DOW. That technique didn’t have a full precision. The first contacts
in 2022 with the European Commission and the EU Customs laboratories led CEN to conclude that the
GC-MS would not be further standardized.
This document has been developed to present a simpler alternative to the market compared to the GC-
MS method. The scope of the method and precision statement will be updated after an interlaboratory
study organized by CEN.
The test method described in this document is based on a standard [2] previously prepared for a former
fuel marker, ACCUTRACE™ S10 ((3-(secbutyl)-4-(decyloxy)phenyl)methanetriyl)tribenzene), which is
used in a few European countries.
prEN 18051:2023 (E)
1 Scope
This document specifies a test method for the determination of the content of n-butyl phenyl ether (BPE,
also known as butoxy-benzene) in gas oils, kerosene, diesel fuel and biodiesel blends. The method uses a
two-column gas chromatograph with an FID-type of detector. The application range is 0,1 mg/l to
21,25 mg/l of BPE, with a limit of detection of 0,05 mg/l.
NOTE This corresponds to 1 % to 150 % of the average marking level of the ACCUTRACE™ Plus required by
Commission Implementing Decision (EU) 2022/197 [1] of 17 January 2022 establishing a common fiscal marker
for gas oils and kerosene.
The method is found to be applicable to determinations beyond this range or for specific other chemical
markers that fall within the distillation temperature range of middle-distillates, but for that no precision
has been determined.
WARNING —The use of this document may 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 to
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)
3 Terms, definitions and abbreviations
3.1 Definitions
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 http://www.iso.org/obp
For the purposes of this document, the following terms and definitions apply:
3.2 Abbreviations
BPE n-butyl phenyl ether
FID flame ionization detector
GC gas chromatograph
LWS linearity working solution
MS mass spectrometry
RF absolute response factor
SCS stock calibration solution
WCS Working calibration solution
prEN 18051:2023 (E)
4 Principle
A test portion is run neat on a multi-dimensional gas-chromatographic system. A pre-separation takes
place on a non-polar pre-column. The middle-distillate part with the ACCUTRACE™ PLUS component is
transferred towards a polar analytical column by using a heart-cut technique. The GC is set towards
optimum flow and temperature setting for the analytical column.
The response areas for the BPE-specific sequential time interval over the entire chromatogram is
determined in a pre-calibration, linearity check step. A flame-ionization detector (FID) is used for
identification and quantification by reference to an external standard using a BPE-free diesel-type fuel.
5 Reagents and materials
5.1 Purity of reagents
Reagent grade chemicals shall be used in all tests.
Any hydrocarbon, oxygen or water present in the gasses used, shall be removed by applying the
appropriate filter.
5.2 Carrier gas, minimum 99,995 %(V/V) purity.
NOTE Helium has been proven to achieve the required level of detection, but hydrogen or nitrogen are options
as well.
...
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