1、PUBLISHED DOCUMENT PD CEN/TR 15160:2005 Petroleum and related products Applicability of diesel fuel test methods for Fatty Acid Methyl Esters (FAME) Information and results on round robin tests ICS 75.160.20 PD CEN/TR 15160:2005 This Published Document was published under the authority of the Standa
2、rds Policy and Strategy Committee on 12 December 2005 BSI 12 December 2005 ISBN 0 580 47336 8 National foreword This Published Document is the official English language version of CEN/TR 15160:2005. The UK participation in its preparation was entrusted to Technical Committee PTI/13, Petroleum testin
3、g and terminology, which has the responsibility to: aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep UK interests informed; monitor related international and European developments
4、and promulgate them in the UK. A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Catalogue under the sec
5、tion entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application.
6、Compliance with a Published Document does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, the CEN/TR title page, pages 2 to 42, an inside back cover and a back cover. The BSI copyright notice displayed in this docum
7、ent indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsTECHNICALREPORT RAPPORTTECHNIQUE TECHNISCHERBERICHT CEN/TR15160 August2005 ICS75.160.20 EnglishVersion PetroleumandrelatedproductsApplicabilityofdieselfueltest methodsforFattyAcidMethylEsters(F
8、AME)Informationand resultsonroundrobintests ProduitsptroliersetproduitsreliApplicationdes mthodesdexaminationdegazoleenMethylAcidesGraz (UMAG)Informationtrsultatsdexaminationinter laboratoir MinerallerzeugnisseundverwandteProdukte AnwendbarkeitvonPrfverfahrenfrDieselKraftstoffeauf FettsureMethyleste
9、r(FAME)Informationenund ErgebnisseausRingversuchen ThisTechnicalReportwasapprovedbyCENon18June2005.IthasbeendrawnupbytheTechnicalCommitteeCEN/TC19. CENmembersarethenationalstandardsbodiesofAustria,Belgium,Cyprus,CzechRepublic,Denmark,Estonia,Finland,France, Germany,Greece,Hungary,Iceland,Ireland,Ita
10、ly,Latvia,Lithuania,Luxembourg,Malta,Netherlands,Norway,Poland,Portugal, Slovakia, Slovenia,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2005CEN Allrightsofexploita
11、tioninanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.CEN/TR15160:2005:E2 Contents Page Foreword 3 Introduction4 1 Summary5 2 Background.5 3 Basis of the work 6 4 Details of the round robin.7 5 Results.7 6 Conclusion 10 Annex A (informative) List of participants in working group
12、26 activities .11 Annex B (informative) Report of the result of the round robin on determination of flash point using the rapid equilibrium close cup method (prEN ISO/DIS 3679)13 Annex C (informative) Report of the result of the round robin series on distillation of petroleum products at reduced pre
13、ssure (ASTM D 1160).20 Annex D (informative) Preliminary study on applicability of distillation of petroleum products at atmospheric pressure (EN ISO 3405) on blends of FAME in diesel fuel25 Annex E (informative) Report of the results of the round robin on determination of carbon residue via the mic
14、ro method (EN ISO 10370).29 Annex F (informative) Report of the result of the round robin series on corrosiveness to copper via the copper strip test (EN ISO 2160).33 Annex G (informative) Report of the result of the round robin series on determination of fatty acid methyl esters (FAME) in middle di
15、stillates via infrared spectroscopy (prEN 14078)36 Annex H (informative) Influence of FAME origin on the measure of FAME content in mineral oil using prEN 14078 (Determination of fatty acid methyl esters (FAME) in middle distillates via infrared spectroscopy method).40 CEN/TR 15160:2005 3 Foreword T
16、his document (CEN/TR 15160:2005) 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 document has been prepared under a mandate given to CEN by the
17、European Commission and the European Free Trade Association. CEN/TR 15160:20054 Introduction This Technical Report gives the results of the round robin series of tests to evaluate different test methods on their compatibility on FAME which are referred to in: EN 14213: Heating fuels Fatty acid methy
18、l esters (FAME) Requirements and test methods, and EN 14214: Automotive fuels Fatty acid methyl esters (FAME) for diesel engines Requirements and test methods. CEN/TC 19 acknowledges Mrs. M.F. Benassy from Total, all project leaders of each test method as indicated in the annexes and all other parti
19、cipants in CEN/TC 19/WG 26 “FAME related fuel test methods“ (see Annex A) for their contribution to this report. CEN/TR 15160:2005 5 1 Summary One task under the European Mandate M/245 was to investigate the applicability of existing petroleum test method standards for fatty acid methyl esters (FAME
20、). For this task CEN/TC 19 has founded a separate working group 26, which has validated 24 methods via round robins, including the development of new test methods. The work of CEN/TC 19/WG 26 was aimed at the drafting of amendments for existing ISO standards (with test methods for fossil fuels). The
21、se amendments include the extension of the scope of the standards to biodiesel as well as the new precision data for biodiesel. To get these new precision data (repeatability & reproducibility), WG 26 has done a major effort to validate all relevant test methods on request of the Task Force of WG 24
22、 and WG 25 dealing with the specifications. 2 Background CEN has been asked by the Commission (Mandate M/245) to elaborate standards for fatty acid methyl esters (FAME) to be used as sole fuel for heating and diesel engines and as an additive to mineral oil based fuels. This work has been divided am
23、ongst two Technical Committees, of which CEN/TC 19 was responsible for determining the applicability of already existing petroleum type test method standards to both pure FAME and to blends. This included comparing precision data, generating new reproducibility and repeatability figures and developi
24、ng new test method standards if necessary. For this task CEN/TC 19 has founded a separate working group with the following task: “Verification of applicability to biodiesel (for use in diesel engines as well as for use as heating oil) of existing test methods (to be validated via round robins) and d
25、evelopment of new test methods, if necessary”. The convenor of this WG 26 was Mrs. Benassy of Total (former ELF Antar), France. For a list of participants in this WG, see Annex A. The work of WG 26 was aimed at the drafting of amendments for existing ISO standards (with test methods for fossil fuels
26、). These amendments include the extension of the scope of the standards to biodiesel as well as the new precision data for biodiesel. To get these new precision data (repeatability & reproducibility), WG 26 has organised several round robin studies. Besides that it had several consultations with oth
27、er WGs responsible for existing or revising of test methods and with the WG 24 (automotive diesel) and WG 25 (heating fuels) dealing with the specifications. Scope of the work was investigating the applicability of each test method towards FAME as 100 % diesel fuel. The repeatability and reproducibi
28、lity were determined if the test method was applicable. Furthermore, it was determined whether the method was also applicable to blends of FAME and diesel fuel. This Technical Report gives an overview of the work of WG 26 and of the results in relation to applicability of each test method and the de
29、termined precision data, giving the basic conclusions and data. A full report with all data per test method has been presented within CEN/TC 19. This report is the basis of two standards: 1. EN 14213:2003, Heating fuels Fatty acid methyl esters (FAME) Requirements and test methods 2. EN 14214:2003,
30、Automotive fuels Fatty acid methyl esters (FAME) for diesel engines Requirements and test methods Moreover, the results of the study by WG 26 have been input in the revision of the automotive diesel fuel specification standard (EN 590). NOTE For the purposes of this document, the terms “% (m/m)” and
31、 “% (V/V)” are used to represent respectively the mass fraction and the volume fraction. CEN/TR 15160:20056 3 Basis of the work The following list of standards 1has been investigated in the period 1999 until 2002: EN 116:1997, Diesel and domestic heating fuels Determination of cold filter plugging p
32、oint EN 590: 1998, Automotive fuels Diesel Requirements and test methods EN 12662:1998, Liquid petroleum products Determination of contamination in middle distillates EN 12634:1998, Petroleum products and lubricants Determination of acid number Non-aqueous potentiometric titration method prEN 14078:
33、2001, Liquid petroleum products Determination of fatty acid methyl esters (FAME) in middle distillates Infrared spectroscopy method EN 22719:1993, Petroleum products and lubricants Determination of flash point - Pensky-Martens closed cup method (ISO 2719:1988) EN 23015:1994, Petroleum products Deter
34、mination of cloud point (ISO 3015:1992) EN ISO 2160:1998, Petroleum products Corrosiveness to copper Copper strip test (ISO 2160:1998) EN ISO 3104:1998/C2:1999, Petroleum products Transparent and opaque liquids Determination of kinematic viscosity and calculation of dynamic viscosity (ISO 3104:1997)
35、 EN ISO 3405:2000, Petroleum products Determination of distillation characteristics at atmospheric pressure (ISO 3405:2000) EN ISO 3675:1998, Crude petroleum and liquid petroleum products Laboratory determination of density Hydrometer method (ISO 3675:1998) prEN ISO/DIS 3679:2001 2) , Petroleum prod
36、ucts - Determination of flash point - Rapid equilibrium closed cup method EN ISO 4259:1995, Petroleum products Determination and application of precision data in relation to methods of test (ISO 4259:1992/Cor.1: 1993) EN ISO 5165:1998, Petroleum products Determination of ignition quality of diesel f
37、uels Cetane engine method (ISO 5165:1998) EN ISO 10370:1995, Petroleum products Determination of carbon residue Micro method (ISO 10370: 1993) EN ISO 12185:1996, Crude petroleum and petroleum products Determination of density Oscillating U-tube method (ISO 12185:1996) EN ISO 12205:1996, Petroleum pr
38、oducts Determination of the oxidation stability of middle distillate fuels (ISO 12205:1995) EN ISO 12937:2000, Petroleum products Determination of water Coulometric Karl Fisher titration method (ISO 12937:2000) 1These standards are referred to in the document as either the EN ISO or the ISO number (
39、given in brackets), but here the correct reference of the actual, updated standard is given. 2 Succeeded by EN ISO 3679:2004, Petroleum products - Determination of flash point - Rapid equilibrium closed cup method (ISO 3679:2004) CEN/TR 15160:2005 7 EN ISO 13759:1996, Petroleum products Determinatio
40、n of alkyl nitrate in diesel fuels Spectrometric method (ISO 13759:1996) EN ISO 14596:1998/C1:1999, Petroleum products Determination of sulfur content Wavelength-dispersive X-ray fluorescence spectrometry (ISO 14596:1998/C1:1999) prEN ISO/DIS 20846:2002, Petroleum products Determination of total sul
41、fur content of liquid petroleum products Ultraviolet Fluorescence Method ISO 3016:1994, Petroleum products Determination of pour point ISO 3987:1994, Petroleum products Lubricating oils and additives Determination of sulfated ash. ISO 6245:2001, Petroleum products Determination of ash ISO 12156-1:19
42、97, Diesel fuels Assessment of lubricity using the high-frequency reproducing rig (HFRR) Part 1: Test method (including Cor. 1:1998) ASTM D 1160:99, Distillation of Petroleum Products at Reduced Pressure 4 Details of the round robin After having considered all existing (statistical) data in the stan
43、dards, WG 26 has decided for which test methods an inter-laboratory study was necessary. For some methods the data were sufficient, for others the decision on applicability was made after internal discussions. For each of the remaining test methods a round robin study was initiated and a project lea
44、der from WG 26 was assigned. The number of participating laboratories changed with each standard, going from 7 to 15. There was a variety in countries but from France, Italy, Austria and Germany there were always laboratories participating. Samples from actual FAME products from different feed-stock
45、s were supplied by ITERG, France. Distribution of the samples, together with the correct protocol, was organised by WG 26. All data received from the labs were statistically treated according to EN ISO 4259. For pure FAME, inter-laboratory testing has been completed for the following determination m
46、ethods 3 : density (EN ISO 3675 and EN ISO 12185), viscosity (EN ISO 3104), flash point (prEN ISO/DIS 3679), sulfur content (EN ISO 20846), carbon residue (EN ISO 10370), cetane number (EN ISO 5165), ash content (ISO 3987), water content (EN ISO 12937), copper corrosion (EN ISO 2160), acid number (E
47、N 12634). For 5 % blends of FAME in diesel fuel only testing on determination of alkyl nitrate content (EN ISO 13759) has been done by WG 26. For sulfur content (five methods) and cetane number (one 5 % blend sample tested among four petroleum type samples) studies have been done by other CEN/TC 19
48、groups, while they were conducting their round robin investigations. 5 Results All results are compiled in Table 1 and Table 2. The conclusions on applicability, repeatability and reproducibility are given for pure FAME and one for blends of 5 % in diesel. The results of the sulfur study on the blends have been left out of the table, as this is part of the report of WG 27. However, their results have been incorporated in the drafting of the
