SIST EN 15470:2008
(Main)Liquefied petroleum gases - Determination of dissolved residues - Gas chromatographic method
Liquefied petroleum gases - Determination of dissolved residues - Gas chromatographic method
This European Standard specifies a method for the determination of the residual matter in liquefied petroleum gases (LPG). The dissolved residue is the amount of organic compounds which is detectable by gas chromatography after evaporation of the sample at ambient temperature and then in an oven at 105°C.The method is not suitable for detecting solid materials nor possibly high molecular weight polymers (> 1 000).This method is being developed as a potential replacement of EN-ISO 13757 method, which would be safer and more environmentally friendly. In addition, this new method is more accurate.The precision data of the method have been determined from 20 mg/kg to 100 mg/kg. For a higher content of residue, the precision has not been tested, but remains of lesser interest as typical specifications are in the range of 20 mg/kg to 100 mg/kg.
Flüssiggase - Bestimmung des gelösten Rückstandes - Gaschromatographisches Verfahren
Diese Europäische Norm beschreibt ein Verfahren zur Bestimmung des gelösten Rückstandes in Flüssiggas (LPG). Der gelöste Rückstand ist die Menge organischer Verbindungen, die mittels Gaschromatographie bestimmbar sind, und zwar nach Verdampfung des Probenteils bei Umgebungstemperatur und anschließend bei 105 °C in einem Trockenschrank.
Das Verfahren ist nicht geeignet zur Bestimmung fester Stoffe oder möglicherweise vorhandener Polymere hohen Molekulargewichts (> 1000).
Der Vorteil des Verfahrens liegt darin, dass nur eine geringe LPG-Menge (50 g bis 75 g) erforderlich ist, und dass verfügbare Qualitätsangaben einen Hinweis ermöglichen auf die Herkunft der Rückstände (Gasöl, Schmierstoffe, Weichmacher usw.).
Dieses Verfahren ist entwickelt worden als möglicher Ersatz der allgemein angewandten Norm EN ISO 13757, sie ist jedoch sicherer und umweltfreundlicher. Außerdem ist dieses neue Verfahren genauer.
WARNUNG — Die Anwendung dieser Norm kann den Einsatz gefährlicher Stoffe, Arbeitsgänge und Geräte mit sich bringen. Diese Norm gibt nicht vor, alle mit ihrer Anwendung verbundenen Sicherheitsprobleme anzusprechen. Der Anwender dieser Norm ist dafür verantwortlich, vorher angemessene Maßnahmen zu ergreifen und die Anwendbarkeit einschränkender Vorschriften zu ermitteln. Alle Arbeiten müssen in einem Abzug durchgeführt werden.
Gaz de pétrole liquéfié - Détermination des résidus dissous - Méthode par chromatographie en phase gazeuse
La présente Norme européenne spécifie une méthode de détermination des matières résiduelles dissoutes dans le gaz de pétrole liquéfié (GPL), dans l’intervalle de 40 mg à 100 mg/kg. Des concentrations plus élevées peuvent être déterminées en ajustant la taille de l’échantillon.
Les résidus dissous sont la quantité de composés organiques détectables par chromatographie en phase gazeuse après évaporation de l’échantillon à température ambiante puis dans une étuve à 105 °C.
Cette méthode ne convient ni à la détection des matières solides ni aux éventuels polymères de masse moléculaire élevée( 1 000g/mol).
Cette méthode est avantageuse car elle ne nécessite qu’une faible quantité de GPL (50 g à 75 g) et les données qualitatives disponibles peuvent fournir des indications sur l’origine des résidus (gas-oil, lubrifiants, plastifiants, etc.).
Cette méthode est développée à titre de remplacement potentiel de la méthode couramment utilisée de l’EN ISO 13757 [1], mais elle est plus sûre et plus respectueuse de l’environnement. Cette nouvelle méthode est en outre plus précise.
Les données de fidélité de cette méthode ont été déterminées de 20 mg/kg à 100 mg/kg. Pour des teneurs plus élevées en résidu, la précision n’a pas été évaluée mais elle se révèle d’un faible intérêt puisque les spécifications classiques s’étendent sur l’intervalle de 20 mg/kg à 100 mg/kg.
NOTE La norme EN 15471 [2] est une méthode gravimétrique qui concerne le même domaine d’application mais avec des valeurs de fidélité légèrement moins bonnes.
AVERTISSEMENT Cette méthode implique des opérations et des matériaux dangereux. Il incombe à l’utilisateur d’établir des règles appropriées de sécurité et de santé. Toute manipulation doit être réalisée sous une hotte fermée.
Utekočinjeni naftni plini – Določevanje raztopljenih ostankov - Metoda plinske kromatografije
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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Liquefied petroleum gases - Determination of dissolved residues - Gas chromatographic methodNURPDWRJUDILMHGaz de pétrole liquéfié - Détermination des résidus dissous - Méthode par chromatographie en phase gazeuseFlüssiggase - Bestimmung des gelösten Rückstandes - Gaschromatographisches VerfahrenTa slovenski standard je istoveten z:EN 15470:2007SIST EN 15470:2008en,de75.160.30ICS:SLOVENSKI
STANDARDSIST EN 15470:200801-februar-2008
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 15470November 2007ICS 75.160.20 English VersionLiquefied petroleum gases - Determination of dissolved residues- High temperature Gas chromatographic methodGaz de pétrole liquéfié - Détermination des résidus dissous- Méthode par chromatographie en phase gazeuse, à hautetempératureFlüssiggase - Bestimmung der gelösten Rückstände -Hochtemperatur-Gaschromatographie-VerfahrenThis European Standard was approved by CEN on 7 October 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 15470:2007: E
EN 15470:2007 (E) 2 Contents Page Foreword.3 1 Scope.4 2 Normative reference.4 3 Terms and definitions.4 4 Principle.4 5 Reagents.5 6 Apparatus.5 7 Test procedure.5 7.1 Safety.5 7.2 Summary of the method.5 7.3 Sampling procedure.6 7.4 Evaporation procedure.6 7.5 Gas Chromatography analysis of the evaporation residue.7 8 Calculations.8 9 Expression of results.8 10 Precision.9 10.1 General.9 10.2 Repeatability, r.9 10.3 Reproducibility, R.9 Annex A (normative)
Equipment for the sampling line and evaporation device.10 A.1 Sampling set.10 A.2 Venting lines.10 Annex B (informative)
Commercial equipment suitable for the method.12 B.1 General.12 B.2 Tube, stainless steel (type 304), ref 30203.12 B.3 Needle valve type SS-SS 2.12 B.4 Gas chromatograph Hewlett Packard 5890.12 B.5 Flasks A1036337.12 B.6 The GC column is a weakly polar capillary column, high temperature, type HT5, supplied by SGE.12 Annex C (informative)
Examples of gas chromatograms.13 Bibliography.15
EN 15470:2007 (E) 3 Foreword This document (EN 15470:2007) 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 May 2008, and conflicting national standards shall be withdrawn at the latest by May 2008. 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. 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 the United Kingdom.
EN 15470:2007 (E) 4 1 Scope This European Standard specifies a method for determining the dissolved residual matter in liquefied petroleum gases (LPG), in the range of 40 mg/kg to 100 mg/kg. Higher concentrations can be determined by adjusting the sample size. The dissolved residue is the amount of organic compounds that are detectable by gas chromatography after evaporation of the sample at ambient temperature and then in an oven at 105 °C. This method is not suitable for detecting solid materials or for possibly high molecular weight polymers
(> 1 000 g/mol). The advantages of this method are that a small quantity of LPG (50 g to 75 g) is required and the qualitative data available may indicate the origin of the residues (gas-oil, lubricants, plasticizers, etc.). This method has been developed as a potential replacement of the commonly used method described in EN ISO 13757 [1], but is safer and more environmentally friendly. In addition, this new method is more accurate. The precision data of the method have been determined from 20 mg/kg to 100 mg/kg. For a higher content of residue, the precision has not been tested, but remains of lesser interest as typical specifications are in the range of 20 mg/kg to 100 mg/kg. NOTE An alternative European Standard, EN 15471 [2], specifies a gravimetric method, which has the same scope and slightly worst fidelity data. WARNING — Use of this method involves hazardous materials and operations. It is the responsibility of the user to establish appropriate safety and health precautions. All handling must be performed in a fume hood. 2 Normative reference 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 ISO 4257, Liquefied petroleum gases - Method of sampling (ISO 4257:2001) 3 Terms and definitions For the purposes of this document, the following term and definition applies. 3.1
liquefied petroleum gas (LPG) petroleum gas that can be stored and/or handled in the liquid phase under moderate conditions of pressure and at ambient temperature, consisting predominantly of propane, butanes, with small proportions of propene, butenes and pentanes/pentenes 4 Principle A known mass of LPG, between 50 g and 75 g, is sampled and evaporated in a standard small glass flask. The residue is heated in an oven at 105 °C for 1 h. It is then diluted with a solvent and one internal standard is added. The mixture is then analyzed by a capillary gas chromatography and quantified by the internal standard method.
EN 15470:2007 (E) 5 5 Reagents 5.1 Isopropylalcohol (IPA), analytical grade. 5.2 Carbon dioxide, solid for cooling. 5.3 Carbon disulfide, analytical grade (99,9 % minimum). 5.4 Normal Octane, analytical grade (99,9 % minimum). 5.5 Pentane, analytical grade (99,5 % minimum). 6 Apparatus 6.1 Sample cylinder, of a total mass compatible with the balance used; preferably made of stainless steel fitted with two stainless steel va
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