1、BSI Standards PublicationBS EN 14078:2014Liquid petroleum products Determination of fatty acidmethyl ester (FAME) contentin middle distillates Infraredspectrometry methodBS EN 14078:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN 14078:2014. Itsupersedes BS
2、 EN 14078:2009/BS 2000-579:2009 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee PTI/13, Petroleum Testing and Terminology.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport
3、to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2014. Published by BSI StandardsLimited 2014ISBN 978 0 580 81183 8ICS 75.160.20Compliance with a British Standard cannot confer immunity fromlegal obligations.Thi
4、s British Standard was published under the authority of theStandards Policy and Strategy Committee on 31 July 2014.Amendments issued since publicationDate Text affectedBS EN 14078:2014EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 14078 May 2014 ICS 75.160.20 Supersedes EN 14078:2009English Ve
5、rsion Liquid petroleum products - Determination of fatty acid methyl ester (FAME) content in middle distillates - Infrared spectrometry method Produits ptroliers liquides - Dtermination de la teneur en esters mthyliques dacides gras (EMAG) des distillats moyens - Mthode par spectromtrie infrarouge F
6、lssige Minerallerzeugnisse - Bestimmung des Gehaltes an Fettsuremethylester (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 con
7、ditions 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 exis
8、ts 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 sta
9、ndards 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, S
10、lovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES 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 reser
11、ved worldwide for CEN national Members. Ref. No. EN 14078:2014 EBS EN 14078:2014EN 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
12、 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 resu
13、lts . 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 BS EN 14078:2014EN 14078:2014 (E) 3 Foreword This document (EN 14078:2014) has been prepar
14、ed 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
15、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 responsib
16、le 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
17、 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
18、, 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
19、United Kingdom. BS EN 14078:2014EN 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 ran
20、ges 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
21、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
22、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
23、 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 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 hazardou
24、s 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 pr
25、ior 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, Liqu
26、id 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
27、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-1is measured. Initially, calibration as well as evaluation of the data
28、 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 dilutio
29、n need to be followed. Measurement should be conducted preferably without dilution for range A and a BS EN 14078:2014EN 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 o
30、ne; 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 th
31、e 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 a
32、s 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 fr
33、ee” 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
34、. 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 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 d
35、ependent 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-1if a cell with a path length of 0,5 mm is used. 6 Sampling and sample han
36、dling 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
37、. 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. Speci
38、fic 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; BS EN 14078:20
39、14EN 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
40、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 det
41、ermined 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 pa
42、th 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 importan
43、t 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 alter
44、native 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
45、shall be recorded and checked for control reasons. The spectrum shall not show signals in the neighbourhood of 1 745 cm-1. 7.3 Selection of the path length 7.3.1 Range A For from approx. 0,05 % (V/V) to approx. 3 % (V/V) cells with a long path length (e.g. KBr) of approx. 0,5 mm, known to the neares
46、t 0,01 mm) have proven to be well suited. Other materials and path lengths are also permissible, though on no account should the path length be chosen less than about 0,2 mm to enable a signal and signal-to-noise ratio as favourable as possible. 7.3.2 Range B For FAME contents from approx. 3 % (V/V)
47、 to approx. 20 % (V/V) a path length of approx. 0,1 mm, known to the nearest 0,01 mm, is recommended in combination with a dilution rate of 1 : 5 (refer to data given in Table A.1). Other cells and path lengths are also possible; however, dilution should be arranged within a comparable dimension in
48、order to avoid any major dilution errors. 7.3.3 Range C For FAME contents above 20 % (V/V), the following measurement parameters are recommended: path length of approx. 0,05 mm, known to the nearest 0,01 mm, with a dilution rate of 1 : 5; path length of approx. 0,1 mm, known to the nearest 0,01 mm,
49、with a dilution rate of 1 : 10. For detailed information refer to data given in Table A.1. BS EN 14078:2014EN 14078:2014 (E) 7 7.4 Calibration 7.4.1 General instructions Calibration and ensuing measurement shall be carried out retaining all other measurement parameters. The lower the FAME content, the smaller is the carbonyl band (even if the absorption intensity is still high) and thus the more critical the background correction. Especially for range A (low FAME contents) the background correction with the calibration samples (and possibly als
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