Liquefied petroleum gases - Determination of dissolved residues - High temperature Gas chromatographic method

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 molar mass polymers (>1 000 g/mol).
From the analysis of a limited LPG sample size (50 g to 75 g) this method allows obtaining information on the potential origin of the residue (gasoil, lubricants, plasticizers, etc.).
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.
NOTE   An alternative European Standard, EN 1547113[1], specifies a gravimetric method.
WARNING - The use of this Standard can involve hazardous materials, operations and equipment. This Standard does not purport to address all of the safety problems associated with its use. It is the responsibility of users of this standard to take appropriate measures to ensure the safety and health of personnel prior to application of the standard, and fulfil statutory and regulatory requirements for this purpose.

Flüssiggas - Bestimmung der gelösten Rückstände - Hochtemperatur-Gaschromatographie-Verfahren

Diese Europäische Norm legt ein Verfahren zur Bestimmung der gelösten Rückstände in Flüssiggas (LPG) im Bereich von 40 mg/kg bis 100 mg/kg fest. Höhere Konzentrationen können durch Anpassung der Probenmenge bestimmt werden.
Der gelöste Rückstand ist die Menge organischer Verbindungen, die nach Verdampfung der Probe bei Umgebungstemperatur und anschließend bei 105 °C in einem Trockenschrank mittels Gaschromatographie nachweisbar sind.
Das Verfahren ist nicht geeignet zur Nachweisbarkeit fester Stoffe oder möglicherweise vorhandener Polymere mit hoher molarer Masse (> 1 000 g/mol).
Durch die Analyse einer begrenzten LPG Probenmenge von 50 g bis 75 g ermöglicht dieses Verfahren Informationen bezüglich der potentiellen Herkunft der Rückstände (Gasöl, Schmierstoffe, Weichmacher usw.) zu erhalten.
Die Präzisionsangaben des Verfahrens wurden für den Bereich von 20 mg/kg bis 100 mg/kg bestimmt. Für höhere Gehalte an Rückständen wurde die Präzision nicht untersucht.
ANMERKUNG   Eine alternative Europäische Norm EN 15471 [1] beschreibt ein gravimetrisches Verfahren.
WARNUNG - Die Anwendung dieser Norm kann die Anwendung gefährlicher Stoffe, Arbeitsgänge und Geräte mit sich bringen. Diese Norm beansprucht nicht, alle damit verbundenen Sicherheits¬probleme zu behandeln. Es liegt in der Verantwortung des Anwenders dieser Norm, vor ihrer 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.

Gaz de pétrole liquéfié - Détermination des résidus dissous - Méthode par chromatographie en phase gazeuse, à haute température

Utekočinjeni naftni plini - Določevanje raztopljenih ostankov - Metoda plinske kromatografije z visoko temperaturo

Revizija preskusne metode za obravnavo varnostnih težav in posodobitev na trenutno najsodobnejše tehnike.
Ta evropski standard določa metodo za določevanje raztopljenih ostankov snovi v utekočinjenih naftnih plinih (LPG) v razponu 40–100 mg/kg. Višje koncentracije je mogoče določiti s prilagajanjem velikosti vzorca.
Raztopljeni ostanki so količina organskih zmesi, ki jih je mogoče zaznati s plinsko kromatografijo po tem, ko vzorec izhlapeva pri temperaturi okolice in nato v peči pri 105 °C.
Ta metoda ni primerna za zaznavanje trdnih materialov ali za polimere z morebitno visoko molekulsko maso
(> 1000 g).
Prednost te metode je v tem, da je potrebna majhna količina utekočinjenega naftnega plina (50–75 g), razpoložljivi kvalitativni podatki pa lahko kažejo na izvor ostankov (plinsko olje, maziva, mehčala itd.).
Ta metoda je bila razvita kot možna zamenjava običajno uporabljene metode, ki je opisana v standardu EN ISO 13757 [1], vendar je varnejša in okolju prijaznejša. Poleg tega je ta nova metoda natančnejša.
Podatki o natančnosti metode so določeni 20–100 mg/kg. Natančnost ni bila preskušena pri večji vsebnosti ostankov, vendar ni tako pomembna, ker so tipične specifikacije v razponu od 20–100 mg/kg.

General Information

Status
Published
Publication Date
04-Jul-2017
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Due Date
05-Jul-2017
Completion Date
05-Jul-2017

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Flüssiggas - Bestimmung der gelösten Rückstände - Hochtemperatur-Gaschromatographie-VerfahrenGaz de pétrole liquéfié - Détermination des résidus dissous - Méthode par chromatographie en phase gazeuse, à haute températureLiquefied petroleum gases - Determination of dissolved residues - High temperature Gas chromatographic method75.160.30Plinska gorivaGaseous fuels71.040.50Fizikalnokemijske analitske metodePhysicochemical methods of analysisICS:Ta slovenski standard je istoveten z:EN 15470:2017SIST EN 15470:2017en,fr,de01-oktober-2017SIST EN 15470:2017SLOVENSKI

STANDARDSIST EN 15470:20081DGRPHãþD
SIST EN 15470:2017
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 15470
July
t r s y ICS
y wä s x rä t r Supersedes EN
s w v y rã t r r yEnglish Version

Liquefied petroleum gases æ Determination of dissolved residues æ High temperature Gas chromatographic methodGaz de pétrole liquéfié æ Détermination des résidus dissous æ Méthode par chromatographie en phase gazeuseá à haute température

Flüssiggas æ Bestimmung der gelösten Rückstände æ HochtemperaturæGaschromatographieæVerfahren This European Standard was approved by CEN on

t v April
t r s yä

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 Serbiaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey and United Kingdomä

EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels

t r s y CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN

s w v y rã t r s y ESIST EN 15470:2017

EN 15470:2017 (E) 2 Contents Page European foreword ................................................................................................................................................................ 3 1 Scope ............................................................................................................................................................................. 4 2 Normative references ............................................................................................................................................. 4 3 Terms and definitions ............................................................................................................................................ 4 4 Principle ...................................................................................................................................................................... 4 5 Reagents ...................................................................................................................................................................... 5 6 Apparatus .................................................................................................................................................................... 5 7 Sampling ...................................................................................................................................................................... 5 8 Procedure.................................................................................................................................................................... 6 8.1 Safety ............................................................................................................................................................................ 6 8.2 Sample transfer procedure ................................................................................................................................... 6 8.3 Evaporation procedure .......................................................................................................................................... 7 8.4 Gas chromatography analysis of the residue ................................................................................................. 7 8.4.1 Preparation of the internal standard solution A .......................................................................................... 7 8.4.2 Determination of the blank .................................................................................................................................. 8 8.4.3 Sample analysis ......................................................................................................................................................... 8 9 Calculations ................................................................................................................................................................ 8 10 Expression of results ............................................................................................................................................... 8 11 Precision ...................................................................................................................................................................... 9 11.1 General ......................................................................................................................................................................... 9 11.2 Repeatability, r .......................................................................................................................................................... 9 11.3 Reproducibility, R .................................................................................................................................................... 9 Annex A (normative)

Equipment for sample transfer and evaporation .......................................................... 10 A.1 Sampling set ............................................................................................................................................................ 10 A.2 Venting lines ........................................................................................................................................................... 10 Annex B (informative)

Examples of gas chromatograms ....................................................................................... 12 Bibliography .......................................................................................................................................................................... 14

SIST EN 15470:2017

EN 15470:2017 (E) 3 European foreword This document (EN 15470:2017) 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 January 2018, and conflicting national standards shall be withdrawn at the latest by January 2018. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN shall not be held responsible for identifying any or all such patent rights. This document supersedes EN 15470:2007. The main changes in this version being: a) numerous changes of both technical and editorial nature have been made to add clarity to the text; b) clarification that the use of a drying agent in the desiccator is not recommended; c) the description of the equipment used has been improved; d) Formula (1) has been corrected for an error; e) small changes in the vent line (6.6) and the flasks (6.7) in order to improve the technical safety of the method; f) information contained in Annex B that deemed to be obsolete has been removed. According to the CEN-CENELEC Internal Regulations, the national standards organisations 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, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. SIST EN 15470:2017

EN 15470:2017 (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 which is 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 molar mass polymers (>1 000 g/mol). From the analysis of a limited LPG sample size (50 g to 75 g) this method allows obtaining information on the potential origin of the residue (gasoil, lubricants, plasticizers, etc.). 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. NOTE An alternative European Standard, EN 15471 [1], specifies a gravimetric method. WARNING — The use of this standard can involve hazardous materials, operations and equipment. This standard does not purport to address all of the safety problems associated with its use. It is the responsibility of users of this standard to take appropriate measures to ensure the 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 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 and butanes, with small proportions of propene, butenes and pentanes/pentenes 4 Principle A known mass of LPG, between 50 g and 75

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