EN 15199-3:2020

Petroleum products - Determination of boiling range distribution by gas chromatography method - Part 3: Crude oil

This document describes 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 crude oils. The boiling range distribution and recovery to C100 or C120 can be determined.
Two procedures are described: single and dual analysis mode. The basis of each is the calculation procedure as described in Annex A.
Procedure A (or Single analysis mode) determines the boiling range through C100 or C120 in a single analysis.
Procedure B (or Dual analysis mode) combines procedure A with the boiling point distribution from C1 up to C9 using the Detailed Hydrocarbon Analysis (DHA) according EN 15199-4. The results of both analyses are merged into one boiling point distribution.
NOTE 1 There is no specific precision statement for the combined results obtained by procedure B. For the precision of the boiling range distribution according to procedure B the precision statements of procedure A and EN 15199-4 apply. No precision has been determined for the results after merging.
NOTE 2 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.
WARNING - 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 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 3: Rohöl

Dieses Dokument beschreibt ein Verfahren zur Bestimmung des Siedeverlaufes in Mineralölerzeugnissen mit Hilfe der Kapillar-Gaschromatographie unter Verwendung eines Flammenionisationsdetektors (FID). Diese Norm ist anwendbar auf Rohöle. Die Bestimmung des Siedeverlaufes und der Wiederfindung kann bis zu C100 oder bis zu C120 vorgenommen werden.
Es werden zwei Verfahren für die Analyse beschrieben, ein Einzelmodus und ein Dualmodus. Für beide gilt das in Anhang A beschriebene Rechenverfahren.
Bei Verfahren A (oder Einzelmodus) wird der Siedebereich durchgehend bis C100 oder C120 mittels einer einzigen Analyse ermittelt.
Verfahren B (oder Dualmodus) kombiniert Verfahren A mit der Siedepunktverteilung von C1 bis zu C9 unter Anwendung der detaillierten Kohlenwasserstoffanalyse (en: Detailed Hydrocarbon Analysis, DHA) nach EN 15199 4. Die Ergebnisse beider Analysen werden in einer Siedepunktverteilung zusammengeführt.
ANMERKUNG 1 Es gibt keine spezielle Präzisionsangabe für die durch Verfahren B erhaltenen kombinierten Ergebnisse. Für die Präzision des Siedeverlaufs nach Verfahren B gelten die Präzisionsangaben von Verfahren A und EN 15199 4. Für die Ergebnisse nach dem Zusammenführen wurde keine Präzision bestimmt.
ANMERKUNG 2 Für die Anwendung 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.
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 im Hinblick auf Sicherheit und Gesundheit zu ergreifen und die Anwendbarkeit einschränkender Vorschriften zu ermitteln.

Produits pétroliers - Détermination de la répartition dans l'intervalle de distillation par méthode de chromatographie en phase gazeuse - Partie 3 : Pétrole brut

Le présent document décrit une méthode pour la détermination de la répartition dans l’intervalle de distillation des produits pétroliers par chromatographie en phase gazeuse capillaire avec détection par ionisation de flamme. Cette norme s’applique aux pétroles bruts. La répartition dans l’intervalle de distillation et la récupération jusqu'à C100 ou C120 peuvent être réalisées.
Deux modes opératoires sont décrits : le mode d’analyse unique et le mode d'analyse double. Ils sont tous deux basés sur la procédure de calcul décrite en Annexe A.
Le mode opératoire A (ou mode d'analyse unique) détermine l’intervalle de distillation jusqu'à C100 ou C120 en une seule analyse.
Le mode opératoire B (ou mode d'analyse double) combine le mode opératoire A avec la répartition des points de distillation de C1 à C9 en utilisant l'analyse détaillée des hydrocarbures (DHA) selon l'EN 15199-4. Les résultats des deux analyses sont fusionnés en une seule répartition des points de distillation.
NOTE 1 Il n'y a pas de fidélité spécifique pour les résultats combinés obtenus selon le mode opératoire B. Pour la fidélité de la répartition dans l’intervalle de distillation selon le mode opératoire B, les valeurs de fidélité établies pour le mode opératoire A et l'EN 15199-4 s'appliquent. Aucune fidélité n'a été déterminée pour les résultats après le fusionnement.
NOTE 2 Pour les besoins du présent document, les termes "% (m/m)" et "% (V/V)" sont utilisés pour représenter respectivement la fraction massique, μ, et la fraction volumique, φ, des produits.
AVERTISSEMENT - L’utilisation du présent document implique 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 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 - 3. del: Surova nafta

General Information

• Status: Published
• Publication Date: 22-Dec-2020
• Withdrawal Date: 29-Jun-2021
• ICS: 75.080 - Petroleum products in general
• Technical Committee: CEN/TC 19 - Petroleum products, lubricants and related products
• Drafting Committee: CEN/TC 19/WG 9 - Chromatographic test methods
• Current Stage: 6060 - Definitive text made available (DAV) - Publishing
• Start Date: 23-Dec-2020
• Due Date: 17-Apr-2021
• Completion Date: 23-Dec-2020
• Ref Project: SIST EN 15199-3:2021 - Petroleum products - Determination of boiling range distribution by gas chromatography method - Part 3: Crude oil

Relations

• Replaces: EN 15199-3:2008 - Petroleum products - Determination of boiling range distribution by gas chromatography method - Part 3: Crude oil
• Effective Date: 08-Jun-2022

Standards Content (Sample)

SLOVENSKI STANDARD
01-marec-2021
Nadomešča:
SIST EN 15199-3:2008
Naftni proizvodi - Določanje porazdelitve območja vrelišč z metodo plinske
kromatografije - 3. del: Surova nafta
Petroleum products - Determination of boiling range distribution by gas chromatography
method - Part 3: Crude oil
Mineralölerzeugnisse - Gaschromatographische Bestimmung des Siedeverlaufes - Teil
3: Rohöle
Produits pétroliers - Détermination de la répartition dans l'intervalle de distillation par
méthode de chromatographie en phase gazeuse - Partie 3: Pétrole brut
Ta slovenski standard je istoveten z: EN 15199-3:2020
ICS:
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
75.040 Surova nafta Crude petroleum
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EN 15199-3
EUROPEAN STANDARD
NORME EUROPÉENNE
December 2020
EUROPÄISCHE NORM
ICS 75.080 Supersedes EN 15199-3:2008
English Version
Petroleum products - Determination of boiling range
distribution by gas chromatography method - Part 3:
Crude oil
Produits pétroliers - Détermination de la répartition Mineralölerzeugnisse - Gaschromatographische
dans l'intervalle de distillation par méthode de Bestimmung des Siedeverlaufes - Teil 3: Rohöle
chromatographie en phase gazeuse - Partie 3 : Pétrole
brut
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 15199-3:2020 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 . 7
6 Apparatus . 10
7 Sampling . 11
8 Preparation of the apparatus . 12
8.1 Gas chromatograph preparation . 12
8.2 System performance check . 12
9 Corrected sample and reference material preparation . 12
10 Calibration . 13
11 Procedure . 15
12 Visual inspection of the chromatograms . 15
12.1 Blank run . 15
12.2 Reference material . 16
12.3 Sample run . 16
13 Calculation . 16
14 Expression of results . 17
15 Precision . 17
15.1 General. 17
15.2 Repeatability . 17
15.3 Reproducibility . 17
16 Test report . 19
Annex A (normative) Calculation procedure . 20
Annex B (informative) Additional guidance for the calculation algorithm . 23
Annex C (normative) System performance check . 27
Annex D (normative) Algorithm for merging boiling point distribution results of EN 15199-3
and EN 15199-4 . 29
Annex E (informative) Boiling points of normal alkanes . 37
Bibliography . 39

European foreword
This document (EN 15199-3:2020) 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 15199-3:2008.
The main changes in this edition are:
—  the algorithm for merging the results of the light end analysis and the simulated distillation analysis
has been added as an informative annex;
—  additional information on the determination of the IBP and FBP is added to help the user to improve
the test results.
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 fraction of crude oil
This document describes the determination of boiling range distribution of materials with initial boiling
points (IBP) below 100 °C and final boiling points (FBP) above 750 °C. For testing materials with initial
boiling points (IBP) above 100 °C and final boiling point (FBP) below 750 °C, Part 1 of the standard may
be used. For testing materials with initial boiling points (IBP) above 100 °C and final boiling point (FBP)
above 750 °C, Part 2 of the standard may be used. Part 4 is used for the determination of the boiling range
distribution of hydrocarbons up to n-nonane in crude oil.
This document is harmonized with IP 545 [6] and ASTM D 7169 [4].
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 describes 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
crude oils. The boiling range distribution and recovery to C or C can be determined.
100 120
Two procedures are described: single and dual analysis mode. The basis of each is the calculation
procedure as described in Annex A.
Procedure A (or Single analysis mode) determines the boiling range through C or C in a
100 120
single analysis.
Procedure B (or Dual analysis mode) combines procedure A with the boiling point distribution from C
up to C using the Detailed Hydrocarbon Analysis (DHA) according EN 15199-4. The results of both
analyses are merged into one boiling point distribution.
NOTE 1 There is no specific precision statement for the combined results obtained by procedure B. For the
precision of the boiling range distribution according to procedure B the precision statements of procedure A and
EN 15199-4 apply. No precision has been determined for the results after merging.
NOTE 2 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.
WARNING — 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 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 15199-4, Petroleum products — Determination of boiling range distribution by gas chromatography
method — Part 4: Light fractions of crude oil
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 https://www.iso.org/obp
NOTE Explanation of some of the terms is given in Figure 1.
3.1
initial boiling point
IBP
temperature corresponding to the retention time at which a net area (3.9) count equal to 0,5 % of the
total sample area (3.8) under the chromatogram is obtained (see Figure 1)

Key
1 start of elution
2 initial boiling point (IBP), 3.1
3 final boiling point (FBP), 3.2
4 end of elution
Figure 1 — Typical chromatogram
3.2
final boiling point
FBP
temperature corresponding to the retention time at which a net area (3.9) count equal to 99,5 % of the
total sample area (3.8) under the chromatogram is obtained (see Figure 1)
Note 1 to entry: If the found recovery is less than 99,5 %, the final boiling point is reported as > 720 °C or > 750 °C
at that recovery.
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 t
...