DIN EN 14078-2014 Liquid petroleum products - Determination of fatty acid methyl ester (FAME) content in middle distillates - Infrared spectrometry method German version EN 14078 2.pdf

1、September 2014 Translation by DIN-Sprachendienst.English price group 11No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).

2、ICS 75.160.20!%:Z“2235855www.din.deDDIN EN 14078Liquid petroleum products Determination of fatty acid methyl ester (FAME) content in middledistillates Infrared spectrometry method;English version EN 14078:2014,English translation of DIN EN 14078:2014-09Flssige Minerallerzeugnisse Bestimmung des Geha

3、ltes an Fettsuremethylester (FAME) in Mitteldestillaten Infrarotspektrometrisches Verfahren;Englische Fassung EN 14078:2014,Englische bersetzung von DIN EN 14078:2014-09Produits ptroliers liquides Dtermination de la teneur en esters mthyliques dacides gras (EMAG) des distillatsmoyens Mthode par spec

4、tromtrie infrarouge;Version anglaise EN 14078:2014,Traduction anglaise de DIN EN 14078:2014-09SupersedesDIN EN 14078:2014-07www.beuth.deIn case of doubt, the German-language original shall be considered authoritative.Document comprises 17 pages 07.14 DIN EN 14078:2014-09 2 A comma is used as the dec

5、imal marker. National 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” (Secretariat: NEN, Netherlands). The responsible German body involved in its prepa

6、ration was the Normenausschuss Materialprfung (DIN Standards Committee Materials Testing), Working Committee NA 062-06-32-01 UA Prfung von FAME of the Fachausschuss Minerall- und Brennstoffnormung (Standardization of petroleum, fuels, lubricants and related products). Attention is brought to the fac

7、t that the text of the warning note given in 7.4.2 should be moved to Clause 1, “Scope” as a normative text (i.e. not as a Note or a “Warning” note) because this warning is a possible restriction of the scope of this standard. The warning note points out that measured results might be inaccurate if

8、the FAME material used for calibration and the FAME material in the analyzed sample are different. In most cases, the mean molecular weight of the FAME material used for calibration is known by the laboratory in question. In cases of doubt, the fatty acid distribution in an unknown diesel sample und

9、er analysis can be determined using DIN EN 14331, and this can then be used to determine the sample s mean molecular weight. The responsible German working committee is working together with CEN/TC 19/JWG 1 to find a suitable way of correcting this problem in this standard. Until this has been done,

10、 interested parties can refer to the following official CEN/TC 19 document for more information on this issue: The CEN/TC 19 document N 1658 can be obtained from Fachausschuss Minerall- und Brennstoffnormung (FAM)1)or directly from DIN Normenausschuss Materialprfung2)upon request. Amendments This st

11、andard differs from DIN EN 14078:2010-04 as follows: a) the test procedure has been updated with an additional range C; b) 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; c) a warning note relating to the FA

12、ME chain length has been added to Subclause 7.4.2. Compared with DIN EN 14078:2014-07, the following correction has been made to the German version only and therefore does not affect the English text: a) in Table 1, line 4 (Middle distillate range C), column 2 (Repeatability) “r = 0,003 2 X - 0,418

13、7” has been replaced by “r = 0,003 2 X + 0,418 7”. Previous editions DIN EN 14078: 2004-03, 2010-04, 2014-07 DIN 51627-1: 2008-08 1)Obtainable from Fachausschuss Minerall- und Brennstoffnormung (FAM), berseering 40, 22297 Hamburg2)Obtainable from DIN Standards Committee Materials Testing (NMP), Am D

14、IN-Platz, Burggrafenstrae 6, 10787 BerlinEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE 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

15、Produits ptroliers liquides - Dtermination de la teneur en esters mthyliques dacides gras (EMAG) des distillats moyens - Mthode par spectromtrie infrarouge Flssige Minerallerzeugnisse - Bestimmung des Gehaltes an Fettsuremethylester (FAME) in Mitteldestillaten - Infrarotspektrometrisches Verfahren T

16、his 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 refere

17、nces 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

18、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,

19、 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 COMIT EUROPEN DE NORMALISATION EUROPISCH

20、ES KOMITEE FR 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 EEN 14078:2014 (E) 2 Contents Foreword 3 1 Scope 4 2 Normative references 4 3 Pr

21、inciple 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

22、 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

23、 for calibration and dilution 12 Bibliography . 15 DINEN 14078:2014-09EN 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

24、 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

25、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

26、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

27、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,

28、 Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 14078:2014-09EN 14078:2014 (E) 4 1 Scope This European Standard specifies a test method for the determination of Fatty Acid Methyl Este

29、r (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/

30、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

31、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 reg

32、ion 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 () of a material. NOTE 2 For conversion of grams FAME

33、 per litre (g FAME/l) to volume fraction, a fixed density for FAME of 883,0 kg/m3is 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 responsibil

34、ity 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 t

35、he 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, Pe

36、troleum 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 p

37、eak maximum of the typical absorption band for esters at about (1 745 5) cm-1is 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

38、,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 DIN EN 14078:2014-09 EN 14078:2014 (E) 5 shorter path

39、 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 im

40、proved 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

41、 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

42、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-pent

43、ane or cyclohexane. 5 Apparatus 5.1 Infrared spectrometer, dispersive or interferometer type, capable of operating in the wave number range from approx. 400 cm-1to 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 mini

44、mum 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)

45、should give an absorbance of about 0,4 at the maximum peak at about 1 745 cm-1if 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 regulati

46、ons 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

47、 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

48、possible and measurement preferably without dilution; range B: shorter path length and dilution adapted to the anticipated FAME content; DIN EN 14078:2014-09 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 oth