EN 15199-1:2020
(Main)Petroleum products - Determination of boiling range distribution by gas chromatography method - Part 1: Middle distillates and lubricating base oils
Petroleum products - Determination of boiling range distribution by gas chromatography method - Part 1: Middle distillates and lubricating base oils
This document specifies a method for the determination of the boiling range distribution of petroleum products by capillary gas chromatography using flame ionization detection. The standard is applicable to materials having a vapour pressure low enough to permit sampling at ambient temperature and a boiling range of at least 100 °C. The standard is applicable to distillates with initial boiling points (IBP) above 100 °C and final boiling points (FBP) below 750 °C, for example, middle distillates and lubricating base stocks.
The test method is not applicable for the analysis of petroleum or petroleum products containing low molecular weight components (for example naphtha’s, reformates, gasolines) or middle distillates like Diesel and Jet fuel.
Petroleum or petroleum products containing blending components which contain heteroatoms (for example alcohols, ethers, acids, or esters) or residue are not to be analysed by this test method.
NOTE For the purposes of this document, the terms "% (m/m)" and "% (V/V)" are used to represent respectively the mass fraction and the volume fraction.
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 standard to establish appropriate safety and health practices and to determine the applicability of regulatory limitations prior to use.
Mineralölerzeugnisse - Gaschromatographische Bestimmung des Siedeverlaufes - Teil 1: Mitteldestillate und Grundöle
Dieses Dokument legt ein Verfahren zur Bestimmung des Siedeverlaufes in Mineralölerzeugnissen mit Hilfe der Kapillar-Gaschromatographie mit einem Flammenionisationsdetektor (FID) fest. Die Norm ist anwendbar auf Mineralölerzeugnisse mit einem für die Probenahme bei Umgebungstemperatur ausreichend niedrigen Dampfdruck und mit einem Siedebereich von mindestens 100 °C. Die Norm ist anwendbar auf Destillate mit einem Siedebeginn (IBP) oberhalb von 100 °C und mit einem Siedeende (FBP) unterhalb von 750 °C, wie z. B. Mitteldestillate und Grundöle.
Das Prüfverfahren ist nicht anzuwenden für die Analyse von Mineralöl oder Mineralölerzeugnissen mit niedermolekularen Anteilen (z. B. Naphtha, Reformat, Ottokraftstoff) oder Mitteldestillaten, wie z. B. Diesel- und Flug-(turbinen-)kraftstoff.
Mineralöl oder Mineralölerzeugnisse, die Blendkomponenten mit Heteroatomen enthalten (z. B. Alkohole, Ether, Säuren oder Ester), oder Rückstände sind mit diesem Prüfverfahren nicht zu untersuchen.
ANMERKUNG Für die Zwecke dieses Dokuments wird zur Angabe des Massenanteils einer Substanz der Ausdruck „% (m/m)“ und für den Volumenanteil einer Substanz der Ausdruck „% (V/V)“ verwendet.
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 dieser Norm, vor der Anwendung angemessene Maßnahmen in Hinblick auf
Produits pétroliers - Détermination de la répartition dans l'intervalle de distillation par méthode de chromatographie en phase gazeuse - Partie 1 : Distillats moyens et huiles lubrifiantes
Le présent document spécifie une méthode de détermination de la répartition dans l’intervalle de distillation des produits pétroliers par chromatographie en phase gazeuse capillaire avec une détection par ionisation de flamme. Il s’applique aux produits dont la pression de vapeur est suffisamment faible pour permettre l’échantillonnage à la température ambiante et dont l’intervalle de distillation est d’au moins 100 °C. Le présent document s’applique aux distillats dont le point d’ébullition initial (IBP) est supérieur à 100 °C et le point d’ébullition final (FBP) est inférieur à 750 °C, par exemple, les distillats moyens et les huiles lubrifiantes.
La méthode d’essai ne s’applique pas pour l’analyse de pétrole ou de produits pétroliers ayant des composants de faible masse moléculaire (par exemple les naphtas, réformats, essences et distillats moyens comme le gazole et le carburéacteur). Les composants contenant des hétero-atomes (par exemple alcools, éthers, acides ou esters) ou les résidus ne peuvent pas être analysés suivant cette méthode.
NOTE Pour les besoins du présent document, les termes "% (m/m)" et "% (V/V)" sont utilisés pour représenter respectivement la fraction massique et la fraction volumique.
AVERTISSEMENT - L’utilisation du présent document peut impliquer l’utilisation de produits, d’opérations et d’équipements à caractère dangereux. Le présent document n’a pas la prétention d’aborder tous les problèmes de sécurité concernés par son usage. Il est de la responsabilité de l’utilisateur de consulter et d’établir des règles de sécurité et d’hygiène appropriées et de déterminer l’applicabilité des restrictions réglementaires avant utilisation.
Naftni proizvodi - Določanje porazdelitve območja vrelišč z metodo plinske kromatografije - 1. del: Srednji destilati in mazalna olja
General Information
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Standards Content (Sample)
SLOVENSKI STANDARD
01-marec-2021
Nadomešča:
SIST EN 15199-1:2006
Naftni proizvodi - Določanje porazdelitve območja vrelišč z metodo plinske
kromatografije - 1. del: Srednji destilati in mazalna olja
Petroleum products - Determination of boiling range distribution by gas chromatography
method - Part 1: Middle distillates and lubricating base oils
Mineralölerzeugnisse - Gaschromatographische Bestimmung des Siedeverlaufes - Teil 1:
Mitteldestillate und Grundöle
Produits pétroliers - Détermination de la répartition dans l'intervalle de distillation par
méthode de chromatographie en phase gazeuse - Partie 1: Distillats moyens et huiles
lubrifiantes
Ta slovenski standard je istoveten z: EN 15199-1:2020
ICS:
75.080 Naftni proizvodi na splošno Petroleum products in
general
75.100 Maziva Lubricants, industrial oils and
related products
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EN 15199-1
EUROPEAN STANDARD
NORME EUROPÉENNE
December 2020
EUROPÄISCHE NORM
ICS 75.080 Supersedes EN 15199-1:2006
English Version
Petroleum products - Determination of boiling range
distribution by gas chromatography method - Part 1:
Middle distillates and lubricating base oils
Produits pétroliers - Détermination de la répartition Mineralölerzeugnisse - Gaschromatographische
dans l'intervalle de distillation par méthode de Bestimmung des Siedeverlaufes - Teil 1:
chromatographie en phase gazeuse - Partie 1 : Distillats Mitteldestillate und Grundöle
moyens et huiles lubrifiantes
This European Standard was approved by CEN on 23 November 2020.
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, 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
© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 15199-1:2020 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 . 6
5 Reagents and materials . 6
6 Apparatus . 9
7 Sampling . 11
8 Preparation of the apparatus . 11
8.1 Gas chromatograph preparation . 11
8.2 System performance check . 11
9 Sample preparation . 11
10 Calibration . 11
11 Procedure. 13
12 Visual inspection of the chromatograms . 14
13 Calculation . 14
14 Expression of results . 14
15 Precision . 14
15.1 General . 14
15.2 Repeatability . 15
15.3 Reproducibility . 15
16 Test report . 16
Annex A (normative) Calculation procedure . 17
Annex B (normative) System performance check . 22
Annex C (normative) Boiling points of n-alkanes . 24
Bibliography . 26
European foreword
This document (EN 15199-1:2020) 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 June 2021, and conflicting national standards shall be
withdrawn at the latest by June 2021.
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 15199-1:2006.
The main changes in this edition are:
— the precision is extended for the recovery points between 10 % and 50 %;
— the text has been updated editorially in order to give better guidance to operators executing the
test.
EN 15199 consists of the following parts, under the general title Petroleum products — Determination of
boiling range distribution by gas chromatography method:
— Part 1: Middle distillates and lubricating base oils;
— Part 2: Heavy distillates and residual fuels;
— Part 3: Crude oil;
— Part 4: Light fractions of crude oil.
This document specifies the determination of boiling range distribution of materials with initial boiling
points (IBP) above 100 °C and final boiling points (FBP) below 750 °C. For testing materials with initial
boiling points (IBP) above 100 °C and final boiling point (FBP) above 750 °C, Part 2 of the standard can
be used. For testing materials with initial boiling points (IBP) below 100 °C and final boiling points
(FBP) above 750 °C, such as crude oils, Part 3 can be used. Part 4 describes the determination of boiling
range distribution of hydrocarbons up to n-nonane in crude oil.
This document is based on IP Test Method IP 480 [4] and ASTM Test Method ASTM D6352 [3].
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, Turkey and the
United Kingdom.
1 Scope
This document specifies a method for the determination of the boiling range distribution of petroleum
products by capillary gas chromatography using flame ionization detection. The standard is applicable
to materials having a vapour pressure low enough to permit sampling at ambient temperature and a
boiling range of at least 100 °C. The standard is applicable to distillates with initial boiling points (IBP)
above 100 °C and final boiling points (FBP) below 750 °C, for example, middle distillates and lubricating
base stocks.
The test method is not applicable for the analysis of petroleum or petroleum products containing low
molecular weight components (for example naphtha’s, reformates, gasolines) or middle distillates like
Diesel and Jet fuel.
Petroleum or petroleum products containing blending components which contain heteroatoms (for
example alcohols, ethers, acids, or esters) or residue are not to be analysed by this test method.
NOTE For the purposes of this document, the terms “% (m/m)” and “% (V/V)” are used to represent
respectively the mass fraction and the volume fraction.
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 standard 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 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:
— ISO Online browsing platform: available at https://www.iso.org/obp
— IEC Electropedia: available at http://www.electropedia.org/
3.1
initial boiling point
IBP
temperature corresponding to the retention time at which a net area counts equal to 0,5 % of the total
sample area (3.6) under the chromatogram is obtained (see Figure 1)
3.2
final boiling point
FBP
temperature corresponding to the retention time at which a net area (3.7) counts equal to 99,5 % of the
total sample area (3.6) under the chromatogram is obtained (see Figure 1)
3.3
area slice
area resulting from the integration of the chromatographic detector signal within a specified retention
time interval
Note 1 to entry: In area slice mode peak detection parameters are bypassed and the detector signal integral is
recorded as area slices of consecutive, fixed duration time interval.
3.4
corrected area slice
area slice (3.3) corrected for baseline offset by subtraction of the exactly corresponding area slice in a
previously recorded blank (non-sample) analysis
3.5
cumulative corrected area
accumulated sum of corrected area slices (3.4) from the beginning of the analysis through a given
retention time, ignoring any non-sample area for example of solvent
3.6
total sample area
cumulative corrected area (3.5), from the initial area point to the final area point, where the
chromatographic signal has returned to baseline after complete sample elution
Key
1 start of elution 4 end of elution
2 IBP (3.1) X retention time (minutes)
3 FBP (3.2) Y Response (pA)
Figure 1 — Typical chromatogram
3.7
net area
cumulative area counts for the sample minus the cumulative area count for the blank
3.8
recovery
ratio of the cumulative area count of the sample to that of the reference material (external standard)
corrected for dilution and material weights combined with the percentage of light ends, if applicable
4 Principle
A test portion is introduced into a gas chromatographic column, which separates hydrocarbons in the
order of increasing boiling point. The column temperature is raised at a linear reproducible rate and the
area under the chromatogram is recorded throughout the analysis. Boiling points are assigned to the
time-axis from a calibration curve obtained by running a mixture o
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