SIST EN 12916:2019
(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 defines 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.
NOTE 1 For the purpose of this European Standard, 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 standard can involve hazardous materials, operations and equipment. This standard does not purport to address all of the safety problems associated with its use. It is the responsibility of users of this standard 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 Brechzahl-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 gilt 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 gilt für paraffinische Dieselkraftstoffe mit bis zu 7 % (V/V) FAME. Dieses Verfahren beinhaltet keine Verdünnung von Proben, damit die geringen Konzentrationen aromatischer Komponenten in diesen Kraftstoffen bestimmt werden können.
Der Gehalt an polyzyklischen aromatischen Kohlenwasserstoffen wird als Summe der Gehalte an diaro-matischen und tri+-aromatischen Kohlenwasserstoffen berechnet; der Gesamtgehalt an aromatischen Kohlenwasserstoffen errechnet sich aus der Summe der individuellen aromatischen Kohlenwasserstofftypen.
Verbindungen, die Schwefel, Stickstoff und Sauerstoff enthalten, können die Bestimmung stören; Mono-alkene stören nicht, während sich vorhandene konjugierte Diene und Polyene störend auswirken können.
ANMERKUNG 1 Für die Zwecke dieser Europäischen Norm 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 charakteris-tischen Elution von der angegebenen Säule für Flüssigchromatographie relativ zu aromatischen Modellverbindungen festgelegt. Die Quantifizierung jeder aromatischen Verbindungsklasse erfolgt durch externe Kalibrierung mit einer einzelnen aromatischen Verbindung für jeden Typ, die für die Aromaten in der Probe repräsentativ sein kann oder nicht. Andere Techniken und Prüfverfahren können die verschiedenen aromatischen Kohlenwasserstoffklassen anders klassifizieren und quantifizieren.
ANMERKUNG 3 Rückspülung ist Teil der laborinternen Wartung.
WARNUNG - Die Anwendung dieser Norm kann die Anwendung gefährlicher Stoffe, Arbeitsgänge und Geräte mit sich bringen. Diese Norm beansprucht nicht, alle damit verbundenen Sicherheitsprobleme zu behandeln. Es liegt in der Verantwortung des Anwenders dieser Norm, vor ihrer Anwendung 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 dans les distillats moyens - Méthode par chromatographie liquide à haute performance avec détection par réfractométrie différentielle
Le présent document prescrit une méthode pour déterminer la teneur en hydrocarbures mono-aromatiques, di-aromatiques, et tri+-aromatiques des carburants diesel, des carburants diesel paraffiniques et des distillats pétroliers.
Le présent document définit deux modes opératoires, A et B.
La procédure A est applicable aux carburants diesel, qui peuvent contenir des esters méthyliques d’acides gras (EMAG) jusqu’à 30 % (V/V) (comme ceux prescrits dans [1], [2] ou [3]), et distillats pétroliers d'intervalle d'ébullition de 150 °C à 400 °C (comme ceux prescrits dans [4]).
La procédure B est applicable aux carburants diesel 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.
NOTE 1 Pour les besoins de la présente Norme 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, la présente Norme 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.
AVERTISSEMENT — L'utilisation de la présente norme peut impliquer la mise en œuvre de produits, d'opérations et d'équipements à caractère dangereux. La présente norme n'est pas censée aborder tous les problèmes de sécurité concernés par son usage. Il est de la responsabilité des utilisateurs de cette norme 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 evropski standard opredeljuje preskusno metodo za določanje vsebnosti monoaromatskih, diaromatskih in tri+-aromatskih ogljikovodikov v dizelskih gorivih, ki lahko vsebujejo do 30-odstotkov (V/V) metilnih estrov maščobnih kislin (FAME), v parafinskih dizelskih gorivih, ki lahko vsebujejo do sedem odstotkov (V/V) metilnih estrov maščobnih kislin, in naftne destilate z območjem vrelišča od 150 °C do 400 °C. Vsebnost policikličnih aromatskih ogljikovodikov je izračunana na podlagi vsote diaromatskih in tri+-aromatskih ogljikovodikov, skupna vsebnost aromatskih spojin pa je izračunana na podlagi vsote posameznih vrst aromatskih ogljikovodikov. Spojine, ki vsebujejo žveplo, dušik in kisik, lahko povzročajo motnje pri določanju; monoalkeni ne povzročajo motenj pri določanju, konjugirani dialkeni in polialkeni pa jih lahko povzročajo, če so prisotni. Izjava o natančnosti postopka A za običajne destilate je bila določena za dizelska goriva s komponentami in brez komponent za mešanje z metilnimi estri maščobnih kislin, ki vsebujejo od šest odstotkov (m/m) do 30 odstotkov (m/m) monoaromatskih spojin, od en odstotek (m/m) do deset odstotkov (m/m) diaromatskih spojin, od 0 odstotkov (m/m) do dva odstotka (m/m) triaromatskih spojin, od en odstotek (m/m) do dvanajst odstotkov (m/m) policikličnih aromatskih spojin in od sedem odstotkov (m/m) do 42 odstotkov (m/m) skupnih aromatskih spojin. Izjava o natančnosti postopka A za nearomatske destilate je bila določena za dizelska goriva s komponentami in brez komponent za mešanje z metilnimi estri maščobnih kislin, ki vsebujejo od 0,2 odstotka (m/m) do 1,8 odstotka (m/m) monoaromatskih spojin, okoli 0,1 odstotka (m/m) diaromatskih in policikličnih aromatskih spojin in od 0,2 odstotka (m/m) do 2 odstotka (m/m) skupnih aromatskih spojin.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-julij-2019
Nadomešča:
SIST EN 12916:2016
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 dans les distillats
moyens - Méthode par chromatographie liquide à haute performance avec détection par
réfractométrie différentielle
Ta slovenski standard je istoveten z: EN 12916:2019
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
May 2019
EUROPÄISCHE NORM
ICS 75.080 Supersedes EN 12916:2016
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 Brechzahl-Detektion
différentielle
This European Standard was approved by CEN on 15 April 2019.
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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey 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
© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 12916:2019 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 . 8
9 Calibration . 11
10 Procedure. 12
10.1 Procedure A for diesel fuels and petroleum distillates . 12
10.2 Procedure B for paraffinic diesel fuels . 12
10.3 Procedure A and B continuation . 12
11 Calculation . 15
11.1 Retention times . 15
11.2 Column resolution . 15
11.3 Cut times . 15
11.4 Aromatic hydrocarbons type content . 16
11.5 Polycyclic and total aromatic hydrocarbons content . 16
12 Expression of results . 16
13 Precision . 16
13.1 General . 16
13.2 Repeatability, r . 17
13.3 Reproducibility, R . 17
14 Test report . 17
Annex A (informative) Column selection and use . 18
Annex B (informative) Practical instructions for paraffinic diesel fuel samples . 19
Bibliography . 20
European foreword
This document (EN 12916:2019) 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 November 2019, and conflicting national standards
shall be withdrawn at the latest by November 2019.
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 12916:2016.
Major change compared to the previous version is the addition of a procedure for the analysis of very
low contents of aromatics in paraffinic diesel fuels. The method now comprises two procedures, A and
B. Procedure A covers diesel fuels and other distillates. Procedure B is set up for paraffinic diesel fuels
which do not require a dilution step. Both procedures have a separate precision statement. Additionally,
the required accuracy of the weighing of the system calibration standards 1 and 2 was increased from
0,001 g to 0,000 1 g.
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, Former Yugoslav Republic of Macedonia,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey 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 defines 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.
NOTE 1 For the purpose of this European Standard, 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 standard can involve hazardous materials, operations and
equipment. This standard does not purport to address all of the safety problems associated with
its use. It is the responsibility of users of this standard 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 http://www.electropedia.org/
— ISO Online browsing platform: available at http://www.iso.org/obp
3.1
non-aromatic hydrocarbon
compound having a shorter retention time on the specified polar column than the majority of mono-
aromatic hydrocarbons
3.2
mono-aromatic hydrocarbon
MAH
compound 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 hydrocarbon
DAH
compound 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 hydrocarbon
T+AH
compound having a longer retention time on the specified polar column than the majority of di-
aromatic hydrocarbons including chrysene
3.5
polycyclic aromatic hydrocarbon
POLY-AH
sum of the di-aromatic hydrocarbons and tri+-aromatic hydrocarbons
3.6
total aromatic hydrocarbon
sum of the mono-aromatic hydrocarbons, di-aromatic hydrocarbons and tri+-aromatic hydrocarbons
Note 1 to entry: Published and unpublished data indicate that the major constituents for each hydrocarbon type
include:
a) non-aromatic hydrocarbons: cyclic and acyclic alkanes (paraffins and naphthenes), mono-alkenes (if
present),
b) MAHs: benz
...
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