SIST EN 15199-4:2015
(Main)Petroleum products - Determination of boiling range distribution by gas chromatography method - Part 4: Light fractions of crude oil
Petroleum products - Determination of boiling range distribution by gas chromatography method - Part 4: Light fractions of crude oil
This European Standard describes a method for the determination of the boiling range distribution of petroleum products by capillary gas chromatography using flame ionisation detection. The standard is applicable to k\light fractions. The boiling range distribution and recovery to C100 or C120 can be determined.
Mineralölerzeugnisse - Gaschromatographische Bestimmung des Siedeverlaufes - Teil 4: Leichte Fraktionen des Rohöls
Diese Europäische Norm beschreibt ein Verfahren zur Bestimmung des Siedeverlaufes von Mineralöl-erzeugnissen mit Hilfe der Kapillar-Gaschromatographie unter Anwendung der Flammenionisationsdetektion. Die Norm ist anwendbar auf stabilisierte Rohöle und gilt für den Siedeverlauf und die Wiederfindung bis einschließlich n Nonan. Ein stabilisiertes Rohöl ist definiert als Öl mit einem Reid-Dampfdruck von höchstens 82,7 kPa.
ANMERKUNG Für die Zwecke dieser Europäischen Norm 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 dieser Europäischen Norm kann den Einsatz gefährlicher Stoffe, Arbeitsgänge und Geräte mit sich bringen. Diese Europäische Norm gibt nicht vor, alle mit ihrer Anwendung verbundenen Sicherheitsprobleme anzusprechen. Der Anwender dieser Norm ist dafür verantwortlich, vorher angemessene Maßnahmen in 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 4 : Lumière fractions du pétrole brut
Naftni proizvodi - Določevanje porazdelitve območja vrelišč z metodo plinske kromatografije - 4. del: Lahke frakcije surovega olja
Ta evropski standard opisuje metodo določevanja porazdelitve območja vrelišč v naftnih proizvodih, in sicer s kapilarno plinsko kromatografijo z zaznavanjem plamenske ionizacije. Standard se uporablja za k\lahke frakcije. Določi se lahko porazdelitev območja vrelišč in obnovitev na C100 ali C120.
General Information
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Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Mineralölerzeugnisse - Gaschromatographische Bestimmung des Siedeverlaufes - Teil 4: Leichte Fraktionen des RohölsProduits pétroliers - Détermination de la répartition dans l'intervalle de distillation par méthode de chromatographie en phase gazeuse - Partie 4 : Lumière fractions du pétrole brutPetroleum products - Determination of boiling range distribution by gas chromatography method - Part 4: Light fractions of crude oil75.080Naftni proizvodi na splošnoPetroleum products in general71.040.50Fizikalnokemijske analitske metodePhysicochemical methods of analysisICS:Ta slovenski standard je istoveten z:EN 15199-4:2015SIST EN 15199-4:2015en,fr,de01-december-2015SIST EN 15199-4:2015SLOVENSKI
STANDARD
SIST EN 15199-4:2015
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 15199-4
September
t r s w ICS
y wä r z r English Version
Petroleum products æ Determination of boiling range distribution by gas chromatography method æ Part
vã Light fractions of crude oil Produits pétroliers æ Détermination de la répartition dans l 5intervalle de distillation par méthode de chromatographie en phase gazeuse æ Partie
v ã Lumière fractions du pétrole brut
Mineralölerzeugnisse æ Gaschromatographische Bestimmung des Siedeverlaufes æ Teil
vã Leichte Fraktionen des Rohöls This European Standard was approved by CEN on
s August
t r s wä
egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä
translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä
CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey andUnited Kingdomä
EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels
9
t r s w CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s w s { {æ vã t r s w ESIST EN 15199-4:2015
EN 15199-4:2015 (E) 2 Contents
page European foreword . 3 1 Scope . 4 2 Normative references . 4 3 Terms and definitions . 4 4 Principle . 4 5 Reagents and materials . 4 6 Apparatus . 5 6.1 Analytical balance . 5 6.2 Gas chromatograph . 5 6.3 Detector . 5 6.4 Pre-column configurations . 5 6.4.1 Heated valve switching box (see Figure B.1). 5 6.4.2 Injection port (see Figure B.2 and B.3) . 6 6.5 Analytical column . 6 6.5.1 General . 6 6.5.2 Resolution . 7 6.6 Skewness . 7 6.7 Data collection . 8 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 . 9 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 . 11 11.3 Reproducibility, R . 11 12 Test report . 12 Annex A (informative)
Analysis assistance . 13 Annex B (informative)
Apparatus configuration . 19 Bibliography . 21
SIST EN 15199-4:2015
EN 15199-4:2015 (E) 3 European foreword This document (EN 15199-4:2015) 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 March 2016, and conflicting national standards shall be withdrawn at the latest by March 2016. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights. 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 part of the standard is based on IP 601 [1] and describes the determination of boiling range distribution of hydrocarbons up to n-nonane in crude oil. The results of this test method can be combined with those from EN 15199-3, to give a full boiling point distribution of crude oil. Part 4 is harmonized with ASTM D7900 [2]. According to the CEN-CENELEC Internal Regulations, the national standards organizations 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, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. SIST EN 15199-4:2015
EN 15199-4:2015 (E) 4 1 Scope This European Standard describes a method for the determination of the boiling range distribution of petroleum products by capillary gas chromatography using flame ionization detection. This European Standard 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]. NOTE For the purposes of this European Standard, the terms “% (m/m)” and “% (V/V)” are used to represent respectively the mass fraction, , and the volume fraction, . WARNING — The use of this European Standard can involve hazardous materials, operations and equipment. This European Standard 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 take appropriate measures to ensure 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, in whole or in part, are normatively referenced in this document and are indispensable for its application. 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. 3.1 recovery combined mass percentages of all light hydrocarbon peaks (except the internal standard peak) in 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 SIST EN 15199-4:2015
EN 15199-4:2015 (E) 5 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, having a baseline resolution from any adjacent eluting peaks (Hexene-1 or 3,3-dimethylbutene-1 (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 disulphide (CS2), purity 99,7 % (V/V) minimum. WARNING — Extremely flammable and toxic by inhalation. 6 Apparatus 6.1 Analytical balance Capable of weighing with an accuracy of 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. 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. 6.3 Detector Flame Ionization Detector 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. 6.4 Pre-column configurations 6.4.1 Heated valve switching box (see Figure B.1) For the isothermal 1 metre pre-column, a heated valve box is needed with its own temperature control. The box will contain an automated six-port valve which is used to back-flush the pre-column. The six-port valve should be made out of material which will not be corroded by the sample (Some crude oils contain high amounts of sulfur components). The valve shall be situated in a heated isothermal oven and be attached to the injector, pre-column, splitter, analytical column and the detector without any cold spots. SIST EN 15199-4:2015
EN 15199-4:2015 (E) 6 6.4.2 Injection port (see Figure B.2 and B.3) A temperature programmable injection port capable of containing a 7,5 cm pre-column, and this
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