SIST EN 15984:2011
(Main)Petroleum industry and products - Determination of composition of refinery heating gas and calculation of carbon content and calorific value - Gas chromatography method
Petroleum industry and products - Determination of composition of refinery heating gas and calculation of carbon content and calorific value - Gas chromatography method
This European Standard specifies a gas chromatographic method to determine individual refinery heating gas components from which carbon content and calorific value can be calculated. The corresponding computational data is included in the standard.
Mineralölindustrie und -produkte - Bestimmung der Zusammensetzung von Heizgas für Raffinerien und Berechnung des Kohlenstoffgehaltes und des Heizwertes - Gaschromatographisches Verfahren
Diese Norm legt ein gaschromatographisches Verfahren für die Untersuchung von Heizgasen fest, wie sie in Raffinerien eingesetzt werden. Mit dem gaschromatographischen Verfahren können insgesamt 23 Bestand-teile von Gasen in Konzentrationen ermittelt werden, wie sie in Raffinerien typischerweise anfallen.
Wasser findet dabei keine Berücksichtigung. Die Ergebnisse beziehen sich auf trockenes Gas.
ANMERKUNG 1 Je nach Verfahren und technischer Ausrüstung des Messplatzes besteht die Möglichkeit, auch höhere Kohlenwasserstoffe auszuweisen.
ANMERKUNG 2 Für die Zwecke dieses Europäischen Norm wird zur Angabe des Volumenanteils (φ) einer Substanz der Ausdruck „% (V/V)“ verwendet.
Industries et produits pétroliers - Détermination de la composition des gaz combustibles de raffinerie, de leur pouvoir calorifique et de leur teneur en carbone - Méthode par chromatographie en phase gazeuse
La présente norme définit une analyse chromatographique pour la détermination des gaz combustibles utilisés dans les raffineries. Cette analyse chromatographique des gaz permet de déterminer 23 composants au total, à des concentrations habituellement trouvées dans les raffineries.
L’eau n’est pas analysée. Les résultats représentent les gaz combustibles à l’état sec.
NOTE 1 Selon la configuration de l’équipement, il est aussi possible de déterminer les hydrocarbures supérieurs.
NOTE 2 Pour les besoins de la présente Norme européenne, les termes “% (V/V)” sont utilisés pour représenter la fraction volumique (φ).
IMPORTANT — La présente norme n'est pas censée 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.
Naftna industrija in proizvodi - Določevanje sestave rafinerijskega kurilnega plina in izračunavanje vsebnosti ogljika in kalorične vrednosti - Plinska kromatografska metoda
Ta evropski standard opredeljuje plinsko kromatografsko metodo za določevanje posameznih sestavin rafinerijskega kurilnega plina, iz katerih je mogoče izračunati vsebnost ogljika in kalorično vrednost. Ustrezni računski podatki so zajeti v standardu.
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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.PHWRGDMineralölindustrie und -produkte - Bestimmung der Zusammensetzung von Heizgas für Raffinerien und Berechnung des Kohlenstoffgehaltes und des Heizwertes - Gaschromatographisches VerfahrenIndustries et produits pétroliers - Détermination de la composition des gaz combustibles de raffinerie, de leur pouvoir calorifique et de leur teneur en carbone - Méthode par chromatographie en phase gazeusePetroleum industry and products - Determination of composition of refinery heating gas and calculation of carbon content and calorific value - Gas chromatography method75.160.30Plinska gorivaGaseous fuelsICS:Ta slovenski standard je istoveten z:EN 15984:2011SIST EN 15984:2011en,fr,de01-julij-2011SIST EN 15984:2011SLOVENSKI
STANDARD
SIST EN 15984:2011
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 15984
April 2011 ICS 75.160 English Version
Petroleum industry and products -Determination of composition of refinery heating gas and calculation of carbon content and calorific value - Gas chromatography method
Industries et produits pétroliers - Détermination de la composition des gaz combustibles de raffinerie, de leur pouvoir calorifique et de leur teneur en carbone - Méthode par chromatographie en phase gazeuse
Mineralölindustrie und -produkte - Bestimmung der Zusammensetzung von Heizgas für Raffinerien und Berechnung des Kohlenstoffgehaltes und des Heizwertes -Gaschromatographisches Verfahren This European Standard was approved by CEN on 9 March 2011.
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, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2011 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15984:2011: ESIST EN 15984:2011
EN 15984:2011 (E) 2 Contents Page Foreword .31 Scope .42 Principle .43 Reagents and materials .44 Apparatus .55 Gas chromatographic analysis .65.1 Analysis systems .65.2 System configuration .65.3 Columns .66 Calibration .76.1 General .76.2 Absolute response factors .76.3 Relative response factors .77 Calculation .87.1 General .87.2 Calculation of the non normalized mole fractions .87.3 Validation of normalized composition (reference components) .87.4 Calculation of carbon content .97.5 Calculation of lower calorific value, on mass basis . 108 Expression of results . 109 Precision . 109.1 General . 109.2 Repeatability . 119.3 Reproducibility . 1110 Test report . 11Annex A (informative)
Possible column combination . 12Annex B (normative)
Detector linearity check . 17Annex C (informative)
Calculation test data . 19Annex D (normative)
Data for calculation. 20Bibliography . 21 SIST EN 15984:2011
EN 15984:2011 (E) 3 Foreword This document (EN 15984:2011) 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 2011, and conflicting national standards shall be withdrawn at the latest by October 2011. 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. This document is based on a DIN Standard [3] with the same scope. 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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. SIST EN 15984:2011
EN 15984:2011 (E) 4 1 Scope This European Standard defines a gas chromatographic analysis for the determination of the composition of fuel gases, as used in refinery heating gas. These results are used to calculate the carbon content and the lower calorific value.
With this gas chromatographic analysis, an overall of 23 refinery heating gas components are determined in concentrations as typically found in refineries (see Table 1 for further details). Water is not analysed. The results represent dry gases. NOTE 1 Depending on the equipment used, there is a possibility to determine higher hydrocarbons as well. NOTE 2 For the purposes of this European Standard, the terms “% (V/V)” is used to represent the volume fraction (3). IMPORTANT — This 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. 2 Principle This standard defines a procedure that is used to determine all components that are present in a typical refinery heating gas, as indicated in Table 1.
NOTE The composition range in which each component can be analyzed does depend on the actual sample composition as higher amounts of a certain component may affect the detection range of other components eluting close by. The general ranges which apply to all the individual components are: Hydrocarbons from 0,01 (mol/100 mol) up to 100 (mol/100 mol); Non-condensable gases from 0,02 (mol/100 mol) up to 100 (mol/100 mol); For hydrogen sulfide a range between 0,1 (mol/100 mol) up to 10 (mol/100 mol) has been found applicable. Three different analysis systems are necessary; they may be built in three separate gas chromatographs, or be integrated into one. Depending on the configuration, hydrocarbons with more than five carbon atoms are reported as a sum parameter. The composition of the refinery heating gas is used to calculate the carbon content and the calorific value. A typical procedure is described hereafter. A configuration is acceptable when the determination gives the precision as described in Clause 9. 3 Reagents and materials 3.1 Gases. 3.1.1 Hydrogen, with a minimum purity of 99,995 % (V/V). 3.1.2 Helium, with a minimum purity of 99,995 % (V/V). 3.1.3 Nitrogen, with a minimum purity of 99,995 % (V/V). 3.1.4 Air, free of oil and water. 3.1.5 Argon, as alternative for analysis system 2, with a minimum purity of 99,995 % (V/V). SIST EN 15984:2011
EN 15984:2011 (E) 5 3.2 Calibration sample. A certified reference gas mixture in concentrations that allow the determination of the necessary response factors (see 6.1) and retention times is required. Table 1 — Refinery heating gas components Number Description Chemical formula 1 Hydrogen H2 2 Oxygen/Argon O2/Ar 3 Nitrogen N2 4 Carbon monoxide CO 5 Carbon dioxide CO2 6 Hydrogen sulfide H2S 7 Methane CH4 8 Ethane C2H6 9 Ethene C2H4 10 Ethyne (Acetylene) C2H2 11 Propane C3H8 12 Propene C3H6 13 Propyne (Methylacetylene) C3H4 14 Propadiene C3H4 15 iso-Butane C4H10 16 n-Butane C4H10 17 trans-2-Butene C4H8 18 1-Butene C4H8 19 2-Methyl-Propene C4H8 20 cis-2-Butene C4H8 21 1,3-Butadiene C4H6 22 iso-Pentane C5H12 23 n-Pentane C5H12 24 Other components with 5 or more Carbon atoms, excluding iso- and n-Pentane (C5+)
4 Apparatus 4.1 Usual laboratory apparatus and glassware. 4.2 Gas chromatographic apparatus, consisting of at least three separation systems able to work simultaneously in one gas chromatograph, with a Thermal Conductivity Detector (TCD) and Flame Ionization Detector (FID) that should be available, and confirming to the requirements as given in Clause 5. SIST EN 15984:2011
EN 15984:2011 (E) 6 5 Gas chromatographic analysis 5.1 Analysis systems The gas chromatographic system consist of the following three parts: 1) Analysis system 1 All components except hydrogen (see Table 1) are retained on a porous polymer and a molecular sieve column and back flushed. NOTE HayeSep© and Molsieve© are examples of such commercially available columns. Hydrogen is determined on a TCD with nitrogen (3.1.3) as the carrier gas (see Figure A.4). 2) Analysis system 2 The second analysis system separates non-condensable gases, carbon dioxide, and hydrocarbons with two carbon atoms and hydrogen sulfide with helium (3.1.2) as the carrier gas and a TCD as a detector. After a pre-separation on a porous polymer column (column 3) propane and higher hydrocarbons are back flushed and vented. See Figure A.5 for details. When the inert gases (O2/Ar, N2, CH4 and CO) are on the molecular sieve 13X column, this column is isolated. Carbon dioxide, the C2-hydrocarbons and hydrogen sulfide are eluted from the porous polymer column (column 4) and are detected. The C2-hydrocarbons from this fraction are not used for quantification. After this the molecular sieve 13X column (column 6) is eluted and the components are determined on the TCD. Methane is quantified on Analysis System 3. 3) Analysis system 3 The third analysis system separates and quantifies all hydrocarbons by an FID and hydrogen (3.1.1) or helium (3.1.2) as the carrier gas. Two columns are used in series. From the methyl silicone column (column 1), the components above a certain cut point e.g. n-pentane are back flushed and determined as a summed peak. The hydrocarbons from the alumina oxide column, column 2, are then separated and quantified. See Figure A.6 for details. 5.2 System configuration The gas chromatographic system may consist of one or more gas chromatographs, with the possibility for isothermal or temperature programmed runs or both depending on the selected system configuration. A TCD and an FID shall be available.
A gas flow control system and gas sampling valves and switching valves are used.
Means for quantification shall be provided. NOTE Optionally a vaporizer may be used. 5.3 Columns A combination of packed and capillary columns is possible.
It shall be ascertained that a quantitative separation of all the components that need to be determined (see Table 1) is possible and that the summed total of C5+ is quantitative. Adequate separation is required between the components on all three separation systems. If cyclopropane can be determined, it shall be summed to propene. An example for a typical configuration is given in Annex A. SIST EN 15984:2011
EN 15984:2011 (E) 7 6 Calibration 6.1 General Depending on the production procedure of the reference gas mixture, it might be necessary to convert the concentration units of the components in the calibration gas to (mol/mol) %. Linearity of the detectors shall be checked according to Annex B. If calibration is necessary, e.g. daily or for an analysis series, a reference gas mixture shall be analysed. For each analysis system (see 5.1) at least one component, the reference component, needs to be calibrated. For example, for analysis system 1 hydrogen, for analysis system 2 nitrogen and for analysis system 3 propane. With these three components, an external calibration is done. The
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