SIST EN 14078:2014
(Main)Liquid petroleum products - Determination of fatty methyl ester (FAME) content in middle distillates - Infrared spectrometry method
Liquid petroleum products - Determination of fatty methyl ester (FAME) content in middle distillates - Infrared spectrometry method
EN 14078 specifies a test method for the determination of Fatty Acid Methyl Ester (FAME) content in diesel fuel or domestic heating fuel by mid infrared spectrometry, which applies to FAME contents of the two measurement ranges as follows: - range A: for FAME contents ranging from approx. 0,05 % (V/V) to approx. 3 % (V/V); - range B: for FAME contents ranging from approx. 3 % (V/V) to approx. 20 % (V/V); - range C: for FAME contents ranging from approx. 20 % (V/V) to approx. 50 % (V/V). Principally, higher FAME contents can also be analyzed if diluted; however, no precision data for results outside the specified range is available at present. This test method was verified to be applicable to samples which contain FAME conforming to EN 14214 or EN 14213. Reliable quantitative results are obtained only if the samples do not contain any significant amounts of other interfering components, especially esters and other carbonyl compounds which possess absorption bands in the spectral region used for quantification of FAME. If such interfering components are present, this test method is expected to produce higher values.
Flüssige Mineralölprodukte - Bestimmung von Fettsäure Methylester (FAME) in Mitteldestillaten - Infrarotspektrometrisches Verfahren
Diese Europäische Norm legt ein Prüfverfahren zur Bestimmung des Gehaltes an Fettsäuremethylestern (FAME, en: Fatty Acid Methyl Esters) in Dieselkraftstoff oder Heizöl mit Hilfe der Infrarotspektrometrie im mittleren Infrarotbereich fest, und zwar für FAME-Gehalte in den drei folgenden Messbereichen:
Messbereich A: für FAME Gehalte von etwa 0,05 % (V/V) bis etwa 3 % (V/V);
Messbereich B: für FAME Gehalte von etwa 3 % (V/V) bis etwa 20 % (V/V);
Messbereich C: für FAME-Gehalte von etwa 20 % (V/V) bis etwa 50 % (V/V).
Höhere FAME-Gehalte können vom Grundsatz her ebenfalls nach entsprechender Verdünnung analysiert werden, jedoch enthält diese Norm gegenwärtig keine Präzisionsangaben für nicht in den genannten Messbereichen liegende Ergebnisse.
Das Prüfverfahren ist anwendbar auf Proben, deren FAME-Anteil die Anforderungsnormen EN 14214 erfüllt. Zuverlässige Ergebnisse können nur dann erhalten werden, wenn die Proben keine signifikanten Anteile an anderen störenden Komponenten enthalten, insbesondere Ester und andere Carbonylverbindungen, die ebenfalls starke Absorptions¬banden im für die FAME-Bestimmung benutzten Spektralbereich aufweisen. Wenn solche Störkomponenten vorhanden sind, wird dieses Prüfverfahren erwartungsgemäß zu hohe FAME Gehalte ausweisen.
ANMERKUNG 1 Für die Zwecke dieses Dokuments wird zur Angabe des Volumenanteils () einer Substanz der Ausdruck „% (VV)“ verwendet.
ANMERKUNG 2 Für die Umrechnung des FAME-Gehaltes von g FAME je Liter (g FAME/l) in „% (VV)“ wird eine mittlere feste Dichte für FAME von 883,0 kg/m3 verwendet.
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 ange-messene¬ Maßnahmen hinsichtlich Sicherheit und Gesundheit zu ergreifen und die Anwendbarkeit einschränkender Vorschriften zu ermitteln.
Produits pétroliers liquides - Détermination de la teneur en esters méthyliques d'acides gras (EMAG) des distillats moyens - Méthode spectrochimique infrarouge
Cette Norme européenne spécifie une méthode d'essai pour la détermination de la teneur en esters méthyliques d'acides gras (EMAG) dans le carburant pour moteurs diesel ou le fioul domestique, par spectrométrie dans l'infrarouge moyen. Cette méthode est applicable pour déterminer des teneurs en EMAG comprises dans l’un des deux intervalles de concentrations suivants :
Intervalle A : pour des teneurs en EMAG comprises entre environ 0,05 % (V/V) et environ 3 % (V/V) ;
Intervalle B : pour des teneurs en EMAG comprises entre environ 3 % (V/V) et environ 20 % (V/V).
Intervalle C : pour des teneurs en EMAG comprises entre environ 20 % (V/V) et environ 50 % (V/V).
En principe, des teneurs en EMAG supérieures peuvent aussi être déterminées par une dilution préalable ; par contre, les données de fidélité ne sont pas disponibles actuellement en dehors des gammes de concentrations mentionnées.
Il a été vérifié que la méthode était applicable à des échantillons contenant des EMAG conformes aux spécifications européennes EN 14214 ou EN 14213 [1]. Des résultats quantitatifs fiables sont obtenus seulement lorsque les échantillons ne contiennent pas d’autres constituants interférant en quantités significatives, en particulier les esters et autres composés carbonylés, qui présentent des bandes d’absorption dans la région spectrale utilisée pour la quantification des EMAG. Lorsque de tels constituants sont présents, cette méthode d’essai donne des valeurs surestimées.
NOTE 1 Pour les besoins de la présente Norme européenne, l'expression «% (V/V)» est utilisée pour représenter la fraction volumique () d'un produit.
NOTE 2 Pour la conversion de grammes d’EMAG par litre (g d’EMAG / l) en fraction volumique, une masse volumique donnée d’EMAG de 883,0 kg/m3 est adoptée.
AVERTISSEMENT — L'utilisation de la présente Norme européenne peut impliquer l'intervention de produits, d'opérations et d'équipements à caractère dangereux. La présente norme européenne n'est pas censée aborder tous les problèmes de sécurité concernés par son usage. Il est de la responsabilité de l'utilisateur de consulter et d'établir des règles de sécurité et d'hygiène appropriées et de déterminer l'applicabilité des restrictions réglementaires avant utilisation.
Tekoči naftni proizvodi - Določevanje metilnih estrov maščobnih kislin (FAME) v srednjih destilatih - Metoda infrardeče spektroskopije
Standard EN 14078 opredeljuje preskusno metodo za določanje vsebnosti metilnih estrov maščobnih kislin (FAME) v dizelskem gorivu ali gorivih za ogrevanje v gospodinjstvih z metodo srednje infrardeče spektroskopije, ki se nanaša na vsebnost metilnih estrov maščobnih kislin dveh razponov merjenja: - razpon A: za vsebnost metilnih estrov maščobnih kislin v razponu od pribl. 0,05 % (V/V) do pribl. 3 % (V/V); - razpon B: za vsebnost metilnih estrov maščobnih kislin v razponu od pribl. 3 % (V/V) do pribl. 20 % (V/V); - razpon C: za vsebnost metilnih estrov maščobnih kislin od pribl. 20 % (V/V) do pribl. 50 % (V/V). Načeloma je možno analizirati tudi višje vsebnosti metilnih estrov maščobnih kislin, če so razredčene; vendar pa trenutno ni na voljo natančnih podatkov za rezultate izven opredeljenega razpona. Ta preskusna metoda je bila potrjena, da se lahko uporablja za vzorce, ki vsebujejo metilne estre maščobnih kislin, v skladu z EN 14214 ali EN 14213. Zanesljive kvantitativne rezultate je mogoče dobiti le, če vzorci ne vsebujejo znatnih količin drugih motečih sestavin, zlasti estrov in drugih karbonilnih spojin, ki imajo absorpcijske pasove v spektralnem območju, ki se uporablja za količinsko določitev metilnih estrov maščobnih kislin. Če so take moteče snovi prisotne, se pričakuje, da bodo vrednosti, pridobljene s to preskusno metodo, višje.
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Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Flüssige Mineralölprodukte - Bestimmung von Fettsäure Methylester (FAME) in Mitteldestillaten - Infrarotspektrometrisches VerfahrenProduits pétroliers liquides - Détermination de la teneur en esters méthyliques d'acides gras (EMAG) des distillats moyens - Méthode spectrochimique infrarougeLiquid petroleum products - Determination of fatty methyl ester (FAME) content in middle distillates - Infrared spectrometry method75.160.20Liquid fuelsICS:Ta slovenski standard je istoveten z:EN 14078:2014SIST EN 14078:2014en,fr,de01-junij-2014SIST EN 14078:2014SLOVENSKI
STANDARDSIST EN 14078:20101DGRPHãþD
SIST EN 14078:2014
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 14078
May 2014 ICS 75.160.20 Supersedes EN 14078:2009English Version
Liquid petroleum products - Determination of fatty acid methyl ester (FAME) content in middle distillates - Infrared spectrometry method
Produits pétroliers liquides - Détermination de la teneur en esters méthyliques d'acides gras (EMAG) des distillats moyens - Méthode par spectrométrie infrarouge
Flüssige Mineralölerzeugnisse - Bestimmung des Gehaltes an Fettsäuremethylester (FAME) in Mitteldestillaten - Infrarotspektrometrisches Verfahren This European Standard was approved by CEN on 10 April 2014.
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, 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 United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2014 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 14078:2014 ESIST EN 14078:2014
EN 14078:2014 (E) 2 Contents Foreword .3 1 Scope .4 2 Normative references .4 3 Principle .4 4 Reagents and materials .5 5 Apparatus .5 6 Sampling and sample handling .5 7 Procedure .5 7.1 Selection and treatment of the cell .5 7.2 Cleaning of the cells .6 7.3 Selection of the path length .6 7.4 Calibration .7 7.5 Sample Preparation .8 7.6 Recording of infrared spectra .8 8 Calculation .9 8.1 Calculation of FAME content in grams per litre (g/l) .9 8.2 Unit conversion from FAME content from g/l to % (V/V) .9 9 Expression of results . 10 10 Precision . 10 10.1 General . 10 10.2 Repeatability, r . 10 10.3 Reproducibility, R . 10 11 Test report . 11 Annex A (informative)
Specific adjustments for calibration and dilution . 12 Bibliography . 15
SIST EN 14078:2014
EN 14078:2014 (E) 3 Foreword This document (EN 14078:2014) 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 November 2014 and conflicting national standards shall be withdrawn at the latest by November 2014. 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 will supersede EN 14078:2009. This third version includes the following significant technical changes with respect to the former: — the test procedure has been updated with an additional range C, and — data from a newly executed Round Robin test have been integrated in order to expand the scope to blends containing up to 50 % (V/V) of FAME. 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 14078:2014
EN 14078:2014 (E) 4 1 Scope This European Standard specifies a test method for the determination of Fatty Acid Methyl Ester (FAME) content in diesel fuel or domestic heating fuel by mid infrared spectrometry, which applies to FAME contents of the three measurement ranges as follows: — range A: for FAME contents ranging from approx. 0,05 % (V/V) to approx. 3 % (V/V); — range B: for FAME contents ranging from approx. 3 % (V/V) to approx. 20 % (V/V); — range C: for FAME contents ranging from approx. 20 % (V/V) to approx. 50 % (V/V). Principally, higher FAME contents can also be analysed if diluted; however, no precision data for results outside the specified range is available at present. This test method was verified to be applicable to samples which contain FAME conforming to EN 14214. Reliable quantitative results are obtained only if the samples do not contain any significant amounts of other interfering components, especially esters and other carbonyl compounds which possess absorption bands in the spectral region used for quantification of FAME. If such interfering components are present, this test method is expected to produce higher values. NOTE 1 For the purposes of this European Standard, the term “% (V/V)” is used to represent the volume fraction (3) of a material. NOTE 2 For conversion of grams FAME per litre (g FAME/l) to volume fraction, a fixed density for FAME of 883,0 kg/m3 is adopted. WARNING — The use of this standard may 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 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 14214, Liquid petroleum products - Fatty acid methyl esters (FAME) for use in diesel engines and heating applications - Requirements and test methods EN ISO 3170, Petroleum liquids - Manual sampling (ISO 3170) EN ISO 3171, Petroleum liquids - Automatic pipeline sampling (ISO 3171) 3 Principle The mid infrared absorption spectrum of a test portion of a sample which is diluted as appropriate if necessary with FAME-free solvent is recorded. The absorbance at the peak maximum of the typical absorption band for esters at about (1 745 ± 5) cm-1 is measured. Initially, calibration as well as evaluation of the data will be carried out as grams FAME per litre. For conversion of grams FAME per litre (g/l) to the reporting unit “% (V/V)”, a fixed density of FAME of 883,0 kg/m3 (at 15 °C) is adopted. Three measurement ranges (A, B or C) have been chosen for which specific adjustments for the calibration and dilution need to be followed. Measurement should be conducted preferably without dilution for range A and a SIST EN 14078:2014
EN 14078:2014 (E) 5 shorter path length of the measurement cell as well as an appropriate dilution for range B and C. In particular, the lower determination range A is a challenging one; all ensuing details shall be kept as a package without any omissions or additions of individual details. That is the only way to adhere to the improved precision data of range A determined by round robin tests. Based on the absorbance measured at the maximum of the peak of the absorption band the FAME content is calculated by means of a calibration function which was determined by measuring calibration solutions for which the FAME content is known. 4 Reagents and materials 4.1 FAME for calibration, FAME as specified in EN 14214. 4.2 FAME free middle distillate as solvent for dilution and as reference material for the measurement of the background spectrum. In particular, a middle distillate suitable for the type of sample (diesel fuel or domestic heating oil) shall be used for range A in order to avoid spectral decompensation as far as possible. In this context, the property “FAME free” means middle distillates without any absorption bands in the IR signal range typical for FAME. 4.3 Solvents for cleaning, such as ethanol, n-pentane or cyclohexane. 5 Apparatus 5.1
Infrared spectrometer, dispersive or interferometer type, capable of operating in the wave number range from approx. 400 cm-1 to approx. 4 000 cm-1, with a linear absorption in the absorbance range from (0,1 to 1,1) absorbance units, and having a resolution of minimum 4 cm-1. 5.2 Cells, made of KBr, NaCl, or CaF2, with known path length, where the additional instructions for the selection and treatment of cells dependent on the applied measurement range as given in 7.1 are followed. EXAMPLE A standard solution with a FAME concentration of 3 g/l (0,34 % (V/V)) should give an absorbance of about 0,4 at the maximum peak at about 1 745 cm-1 if a cell with a path length of 0,5 mm is used. 6 Sampling and sample handling Samples shall be taken according to EN ISO 3170 or EN ISO 3171 as well as in accordance with the requirements of national standards or regulations for the sampling of the product under test. If samples are not tested immediately, they shall be stored tightly sealed and in a cool and dark place. 7 Procedure 7.1 Selection and treatment of the cell The path length of the cell (5.2) shall be selected so that adequate net signal intensities can be obtained (in at least two decimal places, see marked cells in Table A.1). Signal intensities shall still be within the linear detector range. Specific adjustments shall be followed (see recommendations given in Table A.1) depending on measurement range A, B or C: — range A: path length as long as possible and measurement preferably without dilution; — range B: shorter path length and dilution adapted to the anticipated FAME content; SIST EN 14078:2014
EN 14078:2014 (E) 6 — range C: shorter path length and a dilution higher than for range B, adapted to the anticipated FAME content. The path length shall be known or determined exactly. If in use for a longer period of time it should be checked more frequently. A specific and individual calibration shall be made for every cell in use, retaining all other measurement parameters for every applied measurement range. The use of several or different cells during the same calibration is not permissible. The very same cell shall be used for calibration and for sample measurement. Only the exactly determined path length applies for the cell in use; nominal data (nominal path length, labelling, nominal spacer data or the like) shall not be used without any adequate control or correction measures. If cells sensitive to water are used the path length shall be checked more frequently. In case the path length has changed, path length determination and calibration shall be carried out anew. 7.2 Cleaning of the cells After every measurement the cell shall be carefully cleaned with a solvent (4.3). This is particularly important after measuring samples with high FAME content and extremely important when the measurement of samples with low FAME contents is prepared. The cell may also be cleaned by rinsing repeatedly with FAME free middle distillate (4.2). In persistent cases cyclohexane may also be used for cleaning (yet not for calibration or dilution purposes) as well as the following alternative cleaning procedure: a) rinse twice with 5 ml n-pentane each time; then b) rinse once with 5 ml ethanol (absolute); then c) rinse once again with 5 ml n-pentane and finally dry with suitable equipment. In case the cleanliness of the cell is in doubt, a reference spectrum of a FAME free sample shall be recorded and checked f
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