EN 12916:2024
(Main)Petroleum products - Determination of aromatic hydrocarbon types in middle distillates - High performance liquid chromatography method with refractive index detection
Petroleum products - Determination of aromatic hydrocarbon types in middle distillates - High performance liquid chromatography method with refractive index detection
This document specifies a test method for the determination of the content of mono-aromatic, di aromatic and tri+-aromatic hydrocarbons in diesel fuels, paraffinic diesel fuels and petroleum distillates.
This document specifies two procedures, A and B.
Procedure A is applicable to diesel fuels that may contain fatty acid methyl esters (FAME) up to 30 % (V/V) (as in [1], [2] or [3]) and petroleum distillates in the boiling range from 150 °C to 400 °C (as in [4].
Procedure B is applicable to paraffinic diesel fuels with up to 7 % (V/V) FAME. This procedure does not contain a dilution of the sample in order to determine the low levels of aromatic components in these fuels.
The polycyclic aromatic hydrocarbons content is calculated from the sum of di-aromatic and tri+-aromatic hydrocarbons and the total content of aromatic compounds is calculated from the sum of the individual aromatic hydrocarbon types.
Compounds containing sulfur, nitrogen and oxygen can interfere in the determination; mono-alkenes do not interfere, but conjugated di-alkenes and poly-alkenes, if present, can do so. The measurement ranges that apply to this method are given in Table 2 and Table 3.
NOTE 1 For the purpose 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.
NOTE 2 By convention, the aromatic hydrocarbon types are defined on the basis of their elution characteristics from the specified liquid chromatography column relative to model aromatic compounds. Their quantification is performed using an external calibration with a single aromatic compound for each of them, which may or may not be representative of the aromatics present in the sample. Alternative techniques and test methods may classify and quantify individual aromatic hydrocarbon types differently.
NOTE 3 Backflush is part of laboratory-internal maintenance.
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 users of this document to take appropriate measures to ensure the safety and health of personnel prior to application of the standard, and fulfil statutory and regulatory requirements for this purpose.
Mineralölerzeugnisse - Bestimmung von aromatischen Kohlenwasserstoffgruppen in Mitteldestillaten - Hochleistungsflüssigkeitschromatographie-Verfahren mit Brechungsindex-Detektion
Dieses Dokument legt ein Prüfverfahren zur Bestimmung des Gehaltes an monoaromatischen, diaromatischen und tri+-aromatischen Kohlenwasserstoffen in Dieselkraftstoffen, paraffinischen Dieselkraftstoffen und Mineralöldestillaten fest.
Dieses Dokument legt zwei Verfahren fest, A und B.
Verfahren A ist anwendbar für Dieselkraftstoffe, die bis zu 30 % (V/V) Fettsäuremethylester (FAME; en: fatty acid methyl ester) (wie in [1], [2] und [3]) sowie Mineralöldestillate im Siedebereich von 150 °C bis 400 °C (wie in [4]) enthalten dürfen.
Verfahren B ist anwendbar für paraffinische Dieselkraftstoffe mit bis zu 7 % (V/V) FAME. Dieses Verfahren arbeitet ohne Verdünnung der Proben, damit die geringen Konzentrationen aromatischer Komponenten in diesen Kraftstoffen bestimmt werden können.
Der Gehalt an polycyclischen aromatischen Kohlenwasserstoffen wird als Summe der Gehalte an diaromatischen und tri+-aromatischen Kohlenwasserstoffen berechnet; der Gesamtgehalt an aromatischen Verbindungen errechnet sich aus der Summe der einzelnen aromatischen Kohlenwasserstofftypen.
Verbindungen, die Schwefel, Stickstoff und Sauerstoff enthalten, können die Bestimmung stören; Monoalkene stören nicht, während sich vorhandene konjugierte Dialkene und Polyalkene störend auswirken können. Die für dieses Verfahren geltenden Messbereiche sind in Tabelle 2 und Tabelle 3 angegeben.
ANMERKUNG 1 Für die Zwecke dieses Dokuments wird zur Angabe des Massenanteils, µ, einer Substanz der Ausdruck „% (m/m)“ und für den Volumenanteil, φ, einer Substanz der Ausdruck „% (V/V)“ verwendet.
ANMERKUNG 2 Vereinbarungsgemäß werden die aromatischen Kohlenwasserstofftypen auf Basis ihrer charakteristischen Elution von der angegebenen Säule für Flüssigchromatographie relativ zu aromatischen Modellverbindungen festgelegt. Die Quantifizierung erfolgt durch externe Kalibrierung mit einer einzelnen aromatischen Verbindung für jeden Typ, die für die Aromaten in der Probe repräsentativ sein kann. Andere Techniken und Prüfverfahren können die verschiedenen aromatischen Kohlenwasserstofftypen anders klassifizieren und quantifizieren.
ANMERKUNG 3 Rückspülung ist Teil der laborinternen Wartung.
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 des Anwenders dieses Dokuments, vor der Anwendung der Norm geeignete Maßnahmen für die Sicherheit und den Gesundheitsschutz des Personals zu ergreifen und dafür Sorge zu tragen, dass behördliche und gesetzliche Maßnahmen eingehalten werden.
Produits pétroliers - Détermination des familles d'hydrocarbures aromatiques dans les distillats moyens - Méthode par chromatographie liquide à haute performance avec détection par réfractométrie différentielle
Le présent document spécifie une méthode pour déterminer la teneur en hydrocarbures mono-aromatiques, di-aromatiques, et tri+-aromatiques des gazoles, des gazoles paraffiniques et des distillats pétroliers.
Le présent document spécifie deux modes opératoires, A et B.
La procédure A est applicable aux gazoles, qui peuvent contenir des esters méthyliques d’acides gras (EMAG) jusqu’à 30 % (V/V) (comme ceux spécifiés dans [1], [2] ou [3]), et distillats pétroliers d'intervalle d'ébullition de 150 °C à 400 °C (comme ceux spécifiés dans [4]).
La procédure B est applicable aux gazoles paraffiniques qui peuvent contenir jusqu’à 7 % (V/V) d’EMAG. Cette procédure n’implique pas d’étape de dilution de l’échantillon afin de déterminer les faibles teneurs en aromatiques dans ces carburants.
La teneur en hydrocarbures aromatiques polycycliques est calculée à partir de la somme des di-aromatiques, et tri+-aromatiques, et la teneur totale en composés aromatiques est calculée à partir de la somme des teneurs des différentes familles de composés aromatiques.
Les composés soufrés, azotés et oxygénés peuvent interférer dans la mesure. Les mono-oléfines n'interfèrent pas, au contraire des dioléfines conjuguées et des polyoléfines qui peuvent interférer, si elles sont présentes. Les intervalles de mesure qui s’appliquent à cette méthode sont donnés dans le Tableau 2 et le Tableau 3.
NOTE 1 Pour les besoins de le présent document européenne, les expressions « % (m/m) » et « % (V/V) » sont utilisées pour désigner respectivement les fractions massiques, µ, et les fractions volumiques, φ, d’un produit.
NOTE 2 Par convention, le présent document définit les familles d’hydrocarbures aromatiques à partir de leurs caractéristiques d’élution dans la colonne de chromatographie liquide prescrite, et par comparaison aux temps d'élution des composés aromatiques servant de modèle. La quantification est effectuée par étalonnage externe avec un seul composé aromatique par famille d’hydrocarbures aromatiques, ce composé pouvant être ou non représentatif des aromatiques présents dans l’échantillon. Il est possible que des techniques et méthodes alternatives classent et quantifient différemment les familles d'hydrocarbures aromatiques.
NOTE 3 Le rétrobalayage fait partie de la maintenance interne au laboratoire.
AVERTISSEMENT — L'utilisation du présent document peut impliquer la mise en œuvre de produits, d'opérations et d'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 présent 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.
Naftni proizvodi - Določevanje aromatskih ogljikovodikov v srednjih destilatih - Metoda tekočinske kromatografije visoke ločljivosti z detekcijo lomnega količnika
Ta dokument določa preskusno metodo za določevanje vsebnosti aromatskih ogljikovodikov z enim, dvema, tremi ali več aromatskimi obroči v dizelskih gorivih, parafinskih dizelskih gorivih in naftnih destilatih.
Ta dokument določa dva postopka, A in B.
Postopek A se uporablja za dizelska goriva, ki lahko vsebujejo do 30 % (V/V) metilnih estrov maščobnih kislin (FAME) (kot v delih [1], [2] ali [3]), in naftne destilate z vreliščem med 150 °C in 400 °C (kot v delu [4]).
Postopek B se uporablja za parafinska dizelska goriva z vsebnostjo metilnih estrov maščobnih kislin do 7 % (V/V). Ta postopek ne vključuje redčenja vzorca za namene ugotavljanja nizke vsebnosti aromatskih snovi v teh gorivih.
Vsebnost policikličnih aromatskih ogljikovodikov se izračuna s seštevanjem aromatskih ogljikovodikov z dvema obročema in aromatskih ogljikovodikov s tremi ali več obroči, skupna vsebnost aromatskih spojin pa na podlagi seštevka posameznih vrst aromatskih ogljikovodikov.
Spojine, ki vsebujejo žveplo, dušik in kisik, lahko povzročajo motnje pri določevanju; monoalkeni ne povzročajo motenj, konjugirani dialkeni in polialkeni pa jih lahko povzročajo, če so prisotni.
OPOMBA 1: V tem evropskem standardu sta uporabljeni oznaki »% (m/m)« in »% (V/V)«, ki označujeta masni delež (µ) oziroma prostorninski delež (φ) materiala.
OPOMBA 2: Po dogovoru so vrste aromatskih ogljikovodikov opredeljene na podlagi njihovih elucijskih lastnosti določene kolone tekočinske kromatografije v primerjavi z modelnimi aromatskimi spojinami. Njihova kvantifikacija se izvede z uporabo zunanjega umerjanja z enojno aromatsko spojino za posamezno vrsto aromatskih ogljikovodikov, ki je lahko reprezentativna za aromatske spojine iz vzorca ali pa tudi ne. Druge tehnike in preskusne metode lahko drugače razvrstijo in kvantificirajo posamezne vrste aromatskih ogljikovodikov.
OPOMBA 3: Povratno izpiranje je del vzdrževanja laboratorijske opreme.
OPOZORILO: Pri uporabi tega standarda so lahko prisotni nevarni materiali, postopki in oprema. Ta standard ne obravnava vseh varnostnih težav, ki se navezujejo na njegovo uporabo. Za sprejetje ustreznih ukrepov za zagotavljanje varnosti in zdravja osebja pred uporabo standarda ter izpolnjevanje zakonskih in regulativnih zahtev za ta namen so odgovorni uporabniki tega standarda.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-maj-2024
Nadomešča:
SIST EN 12916:2019+A1:2022
Naftni proizvodi - Določevanje aromatskih ogljikovodikov v srednjih destilatih -
Metoda tekočinske kromatografije visoke ločljivosti z detekcijo lomnega količnika
Petroleum products - Determination of aromatic hydrocarbon types in middle distillates -
High performance liquid chromatography method with refractive index detection
Mineralölerzeugnisse - Bestimmung von aromatischen Kohlenwasserstoffgruppen in
Mitteldestillaten - Hochleistungsflüssigkeitschromatographie-Verfahren mit Brechzahl-
Detektion
Produits pétroliers - Détermination des familles d'hydrocarbures aromatiques dans les
distillats moyens - Méthode par chromatographie liquide à haute performance avec
détection par réfractométrie différentielle
Ta slovenski standard je istoveten z: EN 12916:2024
ICS:
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
75.080 Naftni proizvodi na splošno Petroleum products in
general
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EN 12916
EUROPEAN STANDARD
NORME EUROPÉENNE
March 2024
EUROPÄISCHE NORM
ICS 75.080 Supersedes EN 12916:2019+A1:2022
English Version
Petroleum products - Determination of aromatic
hydrocarbon types in middle distillates - High
performance liquid chromatography method with
refractive index detection
Produits pétroliers - Détermination des familles Mineralölerzeugnisse - Bestimmung von aromatischen
d'hydrocarbures aromatiques dans les distillats Kohlenwasserstoffgruppen in Mitteldestillaten -
moyens - Méthode par chromatographie liquide à Hochleistungsflüssigkeitschromatographie-Verfahren
haute performance avec détection par réfractométrie mit Brechungsindex-Detektion
différentielle
This European Standard was approved by CEN on 14 December 2023.
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
© 2024 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 12916:2024 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 5
4 Principle . 6
5 Reagents and materials . 6
6 Apparatus . 7
7 Sampling . 8
8 Apparatus preparation . 9
9 Calibration . 11
10 Procedure. 13
10.1 Procedure A for diesel fuels and petroleum distillates . 13
10.2 Procedure B for paraffinic diesel fuels . 13
10.3 Procedure A and B continuation . 13
11 Calculation . 15
11.1 Retention times . 15
11.2 Column resolution . 16
11.3 Cut times . 16
11.4 Aromatic hydrocarbons type content . 16
11.5 Polycyclic and total aromatic hydrocarbons content . 17
12 Expression of results . 17
13 Precision . 17
13.1 General . 17
13.2 Repeatability, r . 17
13.3 Reproducibility, R . 17
14 Test report . 18
Annex A (informative) Column selection and use . 19
Annex B (informative) Practical instructions for paraffinic diesel fuel samples . 20
Annex C (informative) Identification of tri+-aromatics . 22
Bibliography . 23
European foreword
This document (EN 12916:2024) 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 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 September 2024, and conflicting national standards shall
be withdrawn at the latest by September 2024.
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 12916:2019+A1:2022.
Major change compared to EN 12916:2019+A1:2022 is the introduction of an Annex C with instructions
on determination of tri+-aromatics and additional sampling requirements. This should improve lab
precision when testing paraffinic diesel products. Next, the practical instructions for these type of
samples in Annex B have been improved and exemplary chromatograms have been introduced. The
instructions on storage precautions after sampling have been restricted to paraffinic diesel products only.
The addition of a calibration procedure with refence material ensures better results for all products.
Furthermore, a study executed in 2021 has delivered confirmation of the published precision for PAH
and DAH for concentration range from (6 – 10) % (m/m).
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 test method for the determination of the content of mono-aromatic, di-
aromatic and tri+-aromatic hydrocarbons in diesel fuels, paraffinic diesel fuels and petroleum distillates.
This document specifies two procedures, A and B.
Procedure A is applicable to diesel fuels that may contain fatty acid methyl esters (FAME) up to
30 % (V/V) (as in [1], [2] or [3]) and petroleum distillates in the boiling range from 150 °C to 400 °C (as
in [4].
Procedure B is applicable to paraffinic diesel fuels with up to 7 % (V/V) FAME. This procedure does not
contain a dilution of the sample in order to determine the low levels of aromatic components in these
fuels.
The polycyclic aromatic hydrocarbons content is calculated from the sum of di-aromatic and tri+-
aromatic hydrocarbons and the total content of aromatic compounds is calculated from the sum of the
individual aromatic hydrocarbon types.
Compounds containing sulfur, nitrogen and oxygen can interfere in the determination; mono-alkenes do
not interfere, but conjugated di-alkenes and poly-alkenes, if present, can do so. The measurement ranges
that apply to this method are given in Table 2 and Table 3.
NOTE 1 For the purpose 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.
NOTE 2 By convention, the aromatic hydrocarbon types are defined on the basis of their elution characteristics
from the specified liquid chromatography column relative to model aromatic compounds. Their quantification is
performed using an external calibration with a single aromatic compound for each of them, which can be
representative of the aromatics present in the sample. Alternative techniques and test methods can classify and
quantify individual aromatic hydrocarbon types differently.
NOTE 3 Backflush is part of laboratory-internal maintenance.
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 users of this document to take appropriate measures to ensure the safety and health of
personnel prior to application of the standard, and fulfil statutory and regulatory requirements for this
purpose.
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 14214, Liquid petroleum products — Fatty acid methyl esters (FAME) for use in diesel engines and
heating applications — Requirements and test methods
EN ISO 1042, Laboratory glassware — One-mark volumetric flasks (ISO 1042)
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 https://www.electropedia.org
— ISO Online browsing platform: available at https://www.iso.org/ob
3.1
non-aromatic hydrocarbons
compounds having a shorter retention time on the specified polar column than the majority of mono-
aromatic hydrocarbons
3.2
mono-aromatic hydrocarbons
MAH
compounds having a longer retention time on the specified polar column than the majority of non-
aromatic hydrocarbons, but a shorter retention time than the majority of di-aromatic hydrocarbons
3.3
di-aromatic hydrocarbons
DAH
compounds having a longer retention time on the specified polar column than the majority of mono-
aromatic hydrocarbons, but a shorter retention time than the majority of tri+-aromatic hydrocarbons
3.4
tri+-aromatic hydrocarbons
T+AH
comp
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.