SIST EN 15553:2007
(Main)Petroleum products and related materials - Determination of hydrocarbon types - Fluorescent indicator adsorption method
Petroleum products and related materials - Determination of hydrocarbon types - Fluorescent indicator adsorption method
This European Standard specifies a fluorescent indicator adsorption method for the determination of hydrocarbon types over the concentration ranges from 5 % (V/V) to 99 % (V/V) aromatic hydrocarbons, 0,3 % (V/V) to 55 % (V/V) olefins, and 1 % (V/V) to 95 % (V/V) saturated hydrocarbons in petroleum fractions that distil below 315 oC. This method may apply to concentrations outside these ranges, but the precision has not been determined.
When samples containing oxygenated blending components are analysed, the hydrocarbon type results can be reported on an oxygenate-free basis or, when the oxygenate content is known, the results can be corrected to a total-sample basis.
This test method is for use with full boiling range products. Cooperative data have established that the precision statement does not apply to petroleum fractions with narrow boiling ranges near the 315 °C limit. Such samples are not eluted properly, and results are erratic.
Samples containing dark-coloured components that interfere with reading the chromatographic bands cannot be analysed.
NOTE 1 The oxygenated blending components methanol, ethanol, tert-butyl methyl ether (MTBE), methyl tert-pentyl ether (TAME) and tert-butyl ethyl ether (ETBE) do not interfere with the determination of hydrocarbon types at concentrations normally found in commercial petroleum blends. These oxygenated compounds are not detected since they elute with the alcohol desorbent. The effects of other oxygenated compounds should be individually verified.
NOTE 2 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 may 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 establish appropriate safety and health practices
Mineralölerzeugnisse und verwandte Produkte - Bestimmung der Kohlenwasserstofftypen - Adsorptionsverfahren mit Fluoreszenz-Indikator
Diese Europäische Norm legt ein Verfahren mit Fluoreszenz-Indikator Adsorption fest für die Bestimmung der nachfolgend genannten Kohlenwasserstofftypen in Mineralölfraktionen, die unterhalb von 315 °C sieden, und zwar für aromatische Kohlenwasserstoffe im Bereich von 5 % (V/V) bis 99 % (V/V), für olefinische Kohlenwasserstoffe im Bereich von 0,3 % (V/V) bis 55 % (V/V) und für gesättigte Kohlenwasserstoffe im Bereich von 1 % (V/V) bis 95 % (V/V).
Das Prüfverfahren kann auch auf Produkte mit Gehalten außerhalb der angegebenen Konzentrationsbereiche angewendet werden, jedoch sind für solche Produkte keine Angaben zur Präzision vorhanden.
Für Proben, die sauerstoffhaltige Verbindungen enthalten, können die Kohlenwasserstofftypen ohne Berücksichtigung der sauerstoffhaltigen Verbindungen, (d. h. bezogen auf den sauerstoffverbindungsfreien Probenanteil) angegeben werden, oder aber, wenn der Gehalt an sauerstoffhaltigen Verbindungen bekannt ist, auch nach entsprechender Umrechnung mit Bezug auf die Gesamtprobe.
Dieses Prüfverfahren kann angewendet werden auf Proben, die den gesamten angegebenen Siedebereich überstreichen. Untersuchungen haben gezeigt, dass die Präzisionsangaben nicht gelten für engsiedende Mineralölfraktionen nahe der angegebenen Grenze von 315 °C. Solche Proben werden nicht ordnungsgemäß eluiert und führen daher zu fehlerhaften Ergebnissen.
Proben, die dunkel gefärbte Komponenten enthalten, welche die Auswertung der chromatographischen Zonen stören, können mit diesem Prüfverfahren nicht untersucht werden.
ANMERKUNG 1 Die sauerstoffhaltigen Blendkomponenten Methanol, Ethanol, tert-Butylmethylether (MTBE), Methyl-tert-pentylether (TAME, tert-Amylmethylether) und tert-Butylethylether (ETBE) stören mit für kommerzielle Kraftstoffmischungen üblichen Gehalten die Bestimmung nicht. Diese Blendkomponenten werden nicht erfasst, weil sie zusammen mit dem Laufmittel eluieren.
Produits pétroliers et produits connexes - Détermination des groups d'hydrocarbures - Méthode par adsorption en présence d'indicateur fluorescent
Naftni proizvodi in sorodni materiali - Določevanje vrste ogljikovodikov - Adsorpcijska metoda s fluorescenčnim indikatorjem
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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Petroleum products and related materials - Determination of hydrocarbon types - Fluorescent indicator adsorption methodProduits pétroliers et produits connexes - Détermination des groups d'hydrocarbures - Méthode par adsorption en présence d'indicateur fluorescentMineralölerzeugnisse und verwandte Produkte - Bestimmung der Kohlenwasserstofftypen - Adsorptionsverfahren mit Fluoreszenz-IndikatorTa slovenski standard je istoveten z:EN 15553:2007SIST EN 15553:2007en;fr;de75.080Naftni proizvodi na splošnoPetroleum products in generalICS:SLOVENSKI
STANDARDSIST EN 15553:200701-junij-2007
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 15553April 2007ICS 75.080 English VersionPetroleum products and related materials - Determination ofhydrocarbon types - Fluorescent indicator adsorption methodProduits pétroliers et produits connexes - Déterminationdes groupes d'hydrocarbures - Méthode par adsorption enprésence d'indicateur fluorescentMineralölerzeugnisse und verwandte Produkte -Bestimmung der Kohlenwasserstofftypen - Adsorptionsverfahren mit Fluoreszenz-IndikatorThis European Standard was approved by CEN on 24 February 2007.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the CEN 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 translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2007 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15553:2007: E
EN 15553:2007 (E) 2 Contents Page Foreword.3 1 Scope.4 2 Normative references.4 3 Terms and definitions.5 4 Principle.5 5 Reagents and materials.5 6 Apparatus.6 7 Sampling and sample handling.9 8 Apparatus preparation.9 9 Procedure.10 10 Calculation.12 11 Expression of results.13 12 Precision.13 12.1 Repeatability, r.13 12.2 Reproducibility, R.13 13 Test report.15 Annex A (normative)
Specification for silica gel.16 Annex B (informative)
Standard adsorption column.17 Bibliography.19
EN 15553:2007 (E) 3 Foreword This document (EN 15553:2007) 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 October 2007, and conflicting national standards shall be withdrawn at the latest by October 2007. This European Standard is based on IP 156/06 [1]. It is developed as an alternative method to ASTM D1319 [2], in which a de-pentanization step is described, which is not used in this European Standard and the EU environment. 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, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EN 15553:2007 (E) 4 1 Scope This European Standard specifies a fluorescent indicator adsorption method for the determination of hydrocarbon types over the concentration ranges from 5 % (V/V) to 99 % (V/V) aromatic hydrocarbons, 0,3 % (V/V) to 55 % (V/V) olefinic hydrocarbons, and 1 % (V/V) to 95 % (V/V) saturated hydrocarbons in petroleum fractions that distil below 315 ºC. This method may be applicable to concentrations outside these ranges, but the precision has not been determined. When samples containing oxygenated blending components are analysed, the hydrocarbon type results can be reported on an oxygenate-free basis or, when the oxygenate content is known, the results can be corrected to a total-sample basis. This test method is for use with full boiling range products. Cooperative data have established that the precision statement does not apply to petroleum fractions with narrow boiling ranges near the 315 °C limit. Such samples are not eluted properly, and results are erratic. Samples containing dark-coloured components that interfere with reading the chromatographic bands cannot be analysed. NOTE 1 The oxygenated blending components methanol, ethanol, tert-butyl methyl ether (MTBE), methyl tert-pentyl ether (TAME) and tert-butyl ethyl ether (ETBE) do not interfere with the determination of hydrocarbon types at concentrations normally found in commercial blends. These oxygenated compounds are not detected since they elute with the alcohol desorbent. The effects of other oxygenated compounds should be individually verified. NOTE 2 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 may 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 establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2 Normative references The following referenced documents are indispensable for the application 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 1601, Liquid petroleum products — Unleaded petrol — Determination of organic oxygenate compounds and total organically bound oxygen content by gas chromatography (O-FID) EN 13132, Liquid petroleum products — Unleaded petrol — Determination of organic oxygenate compounds and total organically bound oxygen content by gas chromatography using column switching EN ISO 3170, Petroleum liquids — Manual sampling (ISO 3170:2004) EN ISO 3171, Petroleum liquids — Automatic pipeline sampling (ISO 3171:1988) EN ISO 3696, Water for analytical laboratory use — Specification and test methods (ISO 3696:1987)
EN 15553:2007 (E) 5 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 saturates saturated hydrocarbons volume percentage of alkanes plus cycloalkanes 3.2 olefins olefinic hydrocarbons volume percentage of alkenes plus cycloalkenes plus some alkadienes 3.3 aromatics aromatic hydrocarbons volume percentage of monocyclic and polycyclic aromatic hydrocarbons plus aromatic olefinic hydrocarbons, some dienes, compounds containing sulfur or nitrogen, or higher-boiling oxygenated compounds 4 Principle Approximately 0,75 ml of sample is introduced into a special glass adsorption column packed with activated silica gel. A small layer of the silica gel contains a mixture of fluorescent dyes. When all the sample has been adsorbed onto the gel, alcohol is added to desorb the sample down the column. The hydrocarbons are separated, according to their adsorption affinities, into aromatics, olefins and saturates. The fluorescent dyes are also separated selectively with the hydrocarbon types, and render the boundaries of the aromatic, olefin and saturate zones visible under ultraviolet light. The volume percentage of each hydrocarbon type is calculated from the length of each zone in the column. 5 Reagents and materials Use only chemicals and reagents of recognised analytical grade and water conforming to grade 3 of EN ISO 3696. 5.1 Silica gel, manufactured to conform to the specifications given in Annex A. NOTE 1 Grace Davison silica gel Grade 923 meets the requirements of this specification. Before use, dry the gel in a shallow vessel at 175 ºC for at least 3 h. Transfer the dried gel to an airtight container while still hot, and protect it from atmospheric moisture. NOTE 2 Some batches of silica gel that otherwise meet specifications have been found to produce olefin-boundary fading. The exact reason for this phenomenon is unknown but will affect accuracy and precision. 5.2 Fluorescent indicator-dyed gel, a standard dyed gel, consisting of a mixture of re-crystallized Petrol Red AB4 and purified portions of olefin and aromatic dyes obtained by chromatographic adsorption following a definite, uniform procedure, and deposited on silica gel1). Store the dyed gel in a dark place under an atmosphere of nitrogen. NOTE When stored under these conditions, dyed gel can have a shelf life of at least five years. It is recommended that portions of the dyed gel be transferred as required to a smaller working vial from which the dyed gel is routinely taken for analyses.
1) A list of suppliers is available from the Energy Institute, London.
EN 15553:2007 (E) 6 5.3 Propan-2-ol, 99 % (V/V) 5.4 3-methylbutan-1-ol, 99 % (V/V) (optional) 5.5 Acetone, reagent grade 5.6 Pressurizing gas, air (or nitrogen) capable of being delivered to the top of the column at controllable pressures over the range from 0 kPa gauge to 103 kPa gauge. NOTE A special valve with possibility to regulate this pressure to ± 2 kPa. (see Error! Reference source not found.2) is advised as common valves do not always have this possibility. 6 Apparatus 6.1 Adsorption column, with precision bore tubing conforming to the specification given in Table 1 and as shown in Figure 1, part b), made of glass and consisting of a charger section with a capillary neck, a separator section and an analyzer section. NOTE For routine/non-specification compliance analysis adsorption columns with standard wall tubing conforming to the specification given in Annex B and as shown in Figure 1, part a), may be used. In addition, the length of a thread of liquid approximately 100 mm long, which shall not vary in length by more than 0,3 mm in any part of the analyzer section.
EN 15553:2007 (E) 7
Table 1 — Precision bore column dimensions and tolerance limits Charger section Inside diameter 12 mm ± 2 mm Overall length 150 mm ± 5 mm Neck section Inside diameter 2 mm ± 0,5 mm Overall length 50 mm ± 5 mm Separator section Inside diameter 5 mm ± 0,5 mm Overall length 190 mm ± 5 mm Analyzer section Inside diameter 1,60 mm to 1,65 mm Overall length 1 200mm ± 30 mm Tip Overall length 30 mm ± 5 mm
EN 15553:2007 (E) 8
Key 1 charger 2 neck 3 separator 4 tip 5 analyzer 6 pressuring gas 7 spherical joint S29 8 pack gel to this level 9 long taper 10 dyed gel 11 zone measuring device (optional) 12 long taper 13 polyvinyl tubing 14 precision bore capillary tubing 15 standard wall tubing 16 spherical joint S13 17 tip drawn out to fine capillary Figure 1 — Adsorption columns with a) standard wall and b) precision bore tubing in analyzer section
EN 15553:2007 (E) 9 Glass-sealing of the various sections to each other shall be done with long-taper connections rather than shouldered connections. The silica gel shall be supported with a small piece of glass wool located between the ball socket of the 12/2 spherical joint and covering the analyzer outlet. The column tip attached to the 12/2 socket shall be approximately 2 mm inside diameter. The ball and socket joints shall be clamped together to ensure that the tip does not tend to slide from a position in a direct line with the analyzer section during the packing and subsequent use of the column. 6.2 Zone-measuring-device Either a metre rule mounted adjacent to the column, fitted with four mov
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