Petroleum products - Determination of boiling range distribution by gas chromatography method - Part 4: Light fractions of crude oil

This document specifies a method for the determination of the boiling range distribution of petroleum products by capillary gas chromatography using flame ionization detection. This document is applicable to stabilized crude oils and for the boiling range distribution and the recovery up to and including n-nonane. A stabilized crude oil is defined as having a Reid Vapour Pressure equivalent to or less than 82,7 kPa as determined by IP 481 [3].
Annex C specifies an algorithm for merging the boiling point distribution results obtained using this method with the results obtained with EN 15199-3. This will result in a boiling range distribution and recovery up to C120.
This precision presented in this document is applicable to the boiling range distribution up to n-nonane. For the precision of the boiling range distribution from n-nonane through C120, see EN 15199-3.
NOTE 1   There is no specific precision statement for the combined results obtained after merging the results of EN 15199-3 and EN 15199-4.
NOTE 2   For the purposes of this document, the terms "% (m/m)" and "% (V/V)" are used to represent respectively the mass fraction, ω, and the volume fraction, φ.
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 document to take appropriate measures to ensure safety and health of personnel prior to application of the document and fulfil statutory and regulatory requirements for this purpose.

Mineralölerzeugnisse - Gaschromatographische Bestimmung des Siedeverlaufes - Teil 4: Leichte Fraktionen des Rohöls

Dieses Dokument legt ein Verfahren zur Bestimmung des Siedeverlaufes in Mineralölerzeugnissen mit Hilfe der Kapillar-Gaschromatographie mit einem Flammenionisationsdetektor (FID) fest. Dieses Dokument ist anwendbar auf stabilisierte Rohöle und gilt für den Siedeverlauf und die Ausbeute bis einschließlich n-Nonan. Ein stabilisiertes Rohöl hat per Definition einen Reid-Dampfdruck von 82,7 kPa oder weniger, bestimmt nach IP 481 [3].
Anhang C legt einen Algorithmus zur Zusammenführung der mit diesem Verfahren erhaltenen Ergebnisse zur Siedepunktverteilung mit den Ergebnissen nach EN 15199 3 fest. Dies führt zu einem Siedeverlauf und einer Ausbeute für Kohlenwasserstoffe bis C120.
Die in diesem Dokument dargestellte Präzision gilt für den Siedeverlauf bis zu n-Nonan. Für die Präzision des Siedeverlaufs von n-Nonan durch C120 siehe EN 15199 3.
ANMERKUNG 1   Es gibt keine spezielle Präzisionsangabe für die nach EN 15199 3 und EN 15199 4 erhaltenen kombinierten Ergebnisse.
ANMERKUNG 2   Für die Zwecke dieses Dokuments wird zur Angabe des Massenanteils ω 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 dieses Dokuments, vor seiner 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 de la répartition dans l'intervalle de distillation par méthode de chromatographie en phase gazeuse - Partie 4 : Fractions légères du pétrole brut

Le présent document spécifie une méthode de détermination de la répartition dans l’intervalle de distillation des produits pétroliers par chromatographie en phase gazeuse (CPG) capillaire avec une détection par ionisation de flamme. Le présent document s’applique aux pétroles bruts stabilisés pour déterminer la répartition dans l'intervalle de distillation ainsi que la récupération jusqu'au n-nonane inclus. Un pétrole brut stabilisé est défini comme ayant une pression de vapeur Reid équivalente à 82,7 kPa ou moins, telle que déterminée selon l’IP 481 [3].
L'Annexe C spécifie un algorithme pour fusionner les résultats de la répartition des points d’ébullition obtenus en suivant cette méthode avec ceux obtenus selon l'EN 15199-3. Cela donne une répartition dans l’intervalle de distillation et une récupération jusqu'au C120.
La fidélité présentée dans le présent document est applicable à la répartition dans l’intervalle de distillation jusqu'au n-nonane. Pour la fidélité de la répartition dans l’intervalle de distillation du n-nonane au C120, voir l’EN 15199 3.
NOTE 1   Il n'y a pas de données de fidélité spécifiques pour les résultats combinés obtenus après la fusion des résultats issus de l'EN 15199-3 et ceux issus de l'EN 15199-4.
NOTE 2   Pour les besoins du présent document, les termes « % (m/m) » et « % (V/V) » sont utilisés pour représenter respectivement la fraction massique, ω, et la fraction volumique, φ.
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 du 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 - Določanje porazdelitve območja vrelišč z metodo plinske kromatografije - 4. del: Lahke frakcije surovega olja

General Information

Status
Not Published
Publication Date
07-Jun-2027
Current Stage
4020 - Submission to enquiry - Enquiry
Start Date
04-Sep-2025
Due Date
20-Jan-2026
Completion Date
04-Sep-2025

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Draft
prEN 15199-4:2025 - BARVE
English language
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Standards Content (Sample)


SLOVENSKI STANDARD
01-september-2025
Naftni proizvodi - Določanje porazdelitve območja vrelišč z metodo plinske
kromatografije - 4. del: Lahke frakcije surovega olja
Petroleum products - Determination of boiling range distribution by gas chromatography
method - Part 4: Light fractions of crude oil
Mineralölerzeugnisse - Gaschromatographische Bestimmung des Siedeverlaufes - Teil
4: Leichte Fraktionen des Rohöls
Produits pétroliers - Détermination de la répartition dans l'intervalle de distillation par
méthode de chromatographie en phase gazeuse - Partie 4 : Fractions légères du pétrole
brut
Ta slovenski standard je istoveten z: prEN 15199-4
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.

DRAFT
EUROPEAN STANDARD
NORME EUROPÉENNE
EUROPÄISCHE NORM
August 2025
ICS 75.080 Will supersede EN 15199-4:2021
English Version
Petroleum products - Determination of boiling range
distribution by gas chromatography method - Part 4: Light
fractions of crude oil
Produits pétroliers - Détermination de la répartition Mineralölerzeugnisse - Gaschromatographische
dans l'intervalle de distillation par méthode de Bestimmung des Siedeverlaufes - Teil 4: Leichte
chromatographie en phase gazeuse - Partie 4 : Fraktionen des Rohöls
Fractions légères du pétrole brut
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
© 2025 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 15199-4:2025 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 . 4
5 Reagents and materials . 5
6 Apparatus . 5
7 Sampling and sample handling . 8
8 Calculation of response factors . 8
9 Procedure . 9
9.1 Sample preparation . 9
9.2 Determination of backflush time . 9
9.2.1 Initial work . 9
9.2.2 Analytical column . 9
9.2.3 Accelerated analytical column . 10
9.3 Sample analysis . 10
9.3.1 Initial work . 10
9.3.2 Calculation of individual components results . 10
9.3.3 Boiling point distribution of fraction up to and including nonane . 11
10 Reporting . 11
11 Precision . 11
11.1 General. 11
11.2 Repeatability, r . 12
11.3 Reproducibility, R . 12
12 Test report . 12
Annex A (informative) Analysis assistance . 13
Annex B (informative) Apparatus configuration . 18
Annex C (informative) Algorithm for merging boiling point distribution results of EN 15199-3
and EN 15199-4 . 20
Bibliography . 28

European foreword
This document (prEN 15199-4:2025) 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 will supersede EN 15199-4:2021.
EN 15199-4:2021:
— The figures under Annex A have been corrected, complemented and improved for better assisting
the user.
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
EN 15199-4 is compatible with IP 601 [1] and ASTM D7900 [2].
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. This document is applicable
to stabilized crude oils and for the boiling range distribution and the recovery up to and including n-
nonane. A stabilized crude oil is defined as having a Reid Vapour Pressure equivalent to or less than
82,7 kPa as determined by IP 481 [3].
Annex C specifies an algorithm for merging the boiling point distribution results obtained using this
method with the results obtained with EN 15199-3. This will result in a boiling range distribution and
recovery up to C120.
This precision presented in this document is applicable to the boiling range distribution up to n-nonane.
For the precision of the boiling range distribution from n-nonane through C120, see EN 15199-3.
NOTE 1 There is no specific precision statement for the combined results obtained after merging the results of
EN 15199-3 and EN 15199-4.
NOTE 2 For the purposes of this document, the terms “% (m/m)” and “% (V/V)” are used to represent
respectively the mass fraction, ω, and the volume fraction, φ.
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 document to take appropriate measures to ensure safety and health of
personnel prior to application of the document 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 ISO 3170, Hydrocarbon 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 terminology 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/obp
3.1
recovery
combined mass percentages of all light hydrocarbon identified in the chromatogram (except the internal
standard peak) of the sample up to and including n-nonane
4 Principle
An amount of internal standard is quantitatively added to an aliquot of the stabilized crude oil. A portion
of this mixture is injected into a pre-column in series via a splitter with a capillary analytical column.
When the n-nonane has quantitatively passed to the analytical column, the pre-column is back-flushed to
vent the higher boiling components. The individual components are identified by comparison with
reference chromatograms and a database of hydrocarbon compounds (see Annex A). The boiling point
distribution and recovery up to and including n-nonane (n-C9) is calculated.
5 Reagents and materials
5.1 Stationary phase for columns, with a bonded polydimethylsiloxane (PDMS) stationary phase for
both the pre-column and the analytical capillary column.
5.2 Compressed gases
5.2.1 Carrier gas, helium or hydrogen of at least 99,995 % (V/V) purity or higher is required. Any
oxygen present shall be removed by a suitable chemical filter.
CAUTION — If hydrogen is used as carrier gas, follow the safety instructions from the GC instrument
manufacturer.
5.2.2 Combustion gases, hydrogen and clean air for the flame ionization detector, and suitable filters
shall be used to ensure adequate gas cleanliness.
5.3 Internal standard (I.S.), having a baseline resolution from any adjacent eluting peaks (Hexene-1
or 3,3-dimethyl-1-butene (99 % pure) have been found to be suitable).
5.4 Valve switching mixture, a qualitative mixture of approximately 1 % (m/m) of each normal alkane
from pentane to decane.
5.5 Carbon disulfide (CS ), purity 99,7 % (V/V) minimum.
WARNING — Extremely flammable and toxic by inhalation.
6 Apparatus
6.1 Analytical balance capable of weighing to the nearest 0,1 mg.
6.2 Gas chromatograph.
The typical operational characteristics of the gas chromatograph are described in Table 1.
Two different pre-column configurations are possible.
The first configuration (A) employs a 1 metre column contained in a temperature-controlled valve box,
separately controlled. The valve box in this configuration is isothermal (see Annex B).
The second configuration (B) is a short pre-column (a packed injection port liner), that fits into the
injection port. The injection port will be temperature programmed (see Annex B).
6.3 Flame ionization detector (FID) with sufficient sensitivity to detect 1 % mass n-heptane with a
peak height of at least 10 % full-scale deflection under the conditions given in the method.
When operating at this sensitivity level, detector stability shall be such that a baseline drift of not more
than 1 % per hour is obtained. The detector shall be connected to the column carefully to avoid any cold
spots. The detector shall be capable of operating at a temperature equivalent to the maximum column
temperature used.
Table 1 —Typical
...

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