DIN EN 16091-2012 Liquid petroleum products - Middle distillates and fatty acid methyl ester (FAME) fuels and blends - Determination of oxidation stability by rapid small scale oxi.pdf

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1、February 2012 Translation by DIN-Sprachendienst.English price group 10No 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).I

2、CS 75.160.20!$y_“1866088www.din.deDDIN EN 16091Liquid petroleum products Middle distillates and fatty acid methyl ester (FAME) fuels and blends Determination of oxidation stability by rapid small scale oxidationmethodEnglish translation of DIN EN 16091:2012-02Flssige Minerallerzeugnisse Mitteldestil

3、lat- und Fettsuremethylesterkraftstoffe und Mischungen Bestimmung der Oxidationsstabilitt mit beschleunigtem Verfahren und kleinerProbenmengeEnglische bersetzung von DIN EN 16091:2012-02Produits ptroliers liquides Destillats moyens, esters mthyliques dacides gras (EMAG) et leurs mlanges Dtermination

4、 de la stabilit loxydation par mthode doxydation acclre petitechelleTraduction anglaise de DIN EN 16091:2012-02www.beuth.deDocument comprises pagesIn case of doubt, the German-language original shall be considered authoritative.1501.12 2 A comma is used as the decimal marker. National foreword This

5、standard 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 preparation was the Normenausschuss Materialprfung (Mater

6、ials Testing Standards Committee), Working Committee NA 062-06-32-01 UA Prfung von FAME of the Fachausschuss Minerall- und Brennstoffnormung (FAM). The DIN Standards corresponding to the International Standard referred to in this document are as follows: EN ISO 3170 DIN EN ISO 3170, DIN 51750-1 and

7、DIN 51750-2 National Annex NA (informative) Bibliography DIN 51750-1, Sampling of petroleum products General information DIN 51750-2, Sampling of liquid petroleum products DIN EN ISO 3170, Petroleum liquids Manual sampling DIN EN 16091:2012-02 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 160

8、91 November 2011 ICS 75.160.20 English Version Liquid petroleum products - Middle distillates and fatty acid methyl ester (FAME) fuels and blends - Determination of oxidation stability by rapid small scale oxidation method Produits ptroliers liquides - Distillats moyens, esters mthyliques dacides gr

9、as (EMAG) et leurs mlanges - Dtermination de la stabilit loxydation par mthode doxydation acclre petite chelle Flssige Minerallerzeugnisse - Mitteldestillat- und Fettsuremethylesterkraftstoffe und Mischungen - Bestimmung der Oxidationsstabilitt mit beschleunigtem Verfahren und kleiner Probenmenge Th

10、is European Standard was approved by CEN on 15 October 2011. 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 refer

11、ences 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

12、 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, France, Germany, Greece, Hungary, Ice

13、land, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenu

14、e Marnix 17, B-1000 Brussels 2011 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16091:2011: EEN 16091:2011 (E) 2 Contents Page Foreword 31 Scope 42 Normative references 43 Terms and definitions .44 Principle 45 Reagents and mater

15、ials 46 Apparatus .56.1 Automatically controlled oxidation tester, comprising an oxidation reaction vessel containing: .56.2 Pipette, capable of delivering 5,0 ml 0,1 ml. 56.3 O-ring seals, see A.6. .57 Sampling and sample handling 58 Performance check of the apparatus.59 Preparation of the apparatu

16、s 610 Procedure .611 Expression of results 712 Precision .712.1 General 712.2 Repeatability, r .712.3 Reproducibility, R 713 Test report 7Annex A (normative) Apparatus description 8A.1 General requirements 8A.2 Assembly of apparatus .8A.3 Reaction vessel 9A.4 Screw cap .9A.5 Electric heater 9A.6 O-r

17、ing seals 9A.7 Valves 9A.8 Pressure sensor .9A.9 Temperature sensor 9A.10 Connecting pipes .9A.11 Cooling fan 10Annex B (informative) Calibration process 11Annex C (informative) Determination of induction period . 12Bibliography . 13DIN EN 16091:2012-02 EN 16091:2011 (E) 3 Foreword This document (EN

18、 16091:2011) 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 publi

19、cation of an identical text or by endorsement, at the latest by May 2012, and conflicting national standards shall be withdrawn at the latest by May 2012. 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 no

20、t be held responsible for identifying any or all such patent rights. 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,

21、 Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. DIN EN 16091:2012-02 EN 16091:2011 (E) 4 1 Scope This European St

22、andard specifies a method for the determination of the oxidation stability of middle distillate fuels, fatty acid methyl ester (FAME) fuel and blends thereof, under accelerated conditions, by measuring the induction period to the specified breakpoint in a reaction vessel charged with the sample and

23、oxygen. NOTE 1 For the purposes of this European Standard, the term “% (V/V)” is used to represent the volume fraction (). NOTE 2 The induction period is used as an indication for the resistance of middle distillates, fatty acid methyl ester (FAME) fuels and blends thereof against oxidation. It shou

24、ld be recognized, however, that this correlation can vary markedly under different conditions with different FAMEs and diesel fuel blends. NOTE 3 The presence of ignition improvers may lead to lower oxidation stability results determined by this method. It has for instance been observed that the add

25、ition of 2-ethyl hexyl nitrate (2EHN) can reduce the measured oxidation stability values. 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

26、 of the referenced document (including any amendments) applies. EN ISO 3170, Petroleum liquids Manual sampling (ISO 3170:2004) EN ISO 3171, Petroleum liquids Automatic pipeline sampling (ISO 3171:1988) 3 Terms and definitions For the purposes of this document, the following terms and definitions app

27、ly. 3.1 breakpoint point in the pressure-time curve, where the pressure in the vessel has dropped 10 % below the maximum pressure achieved in the current test run 3.2 induction period time elapsed between starting the heating procedure of the reaction vessel, charged with sample and oxygen, and the

28、breakpoint at 140 C 4 Principle At ambient temperature, a known volume of a sample is placed in a reaction vessel charged with oxygen to a pressure of 700 kPa 5 kPa. The reaction vessel is heated to 140 C. The pressure in the vessel drops as the oxygen is consumed during the oxidation of the sample.

29、 The pressure in the vessel is recorded at intervals of 1s until the breakpoint is reached. The elapsed time from start to the breakpoint is the induction period at the test temperature of 140 C 0,5 C. 5 Reagents and materials 5.1 Cleaning solvent, for the removal of oxidation residues from the test

30、 vessel, of suitable purity to leave no residue on the apparatus. NOTE Commercially available ethanol of approx. 95 % (V/V) purity was found to be suitable. DIN EN 16091:2012-02 EN 16091:2011 (E) 5 5.2 Oxygen, extra dry ( 5 mg/kg water), commercially available, with a purity of not less than 99,6 %.

31、 5.3 Cleaning tissues, lint-free for cleaning sensitive galvanic coated surfaces without scratching. 5.4 Verification fluid, hydrocarbon fuel (B0). NOTE Any hydrocarbon fuel with sufficient stability and a known induction period may be used as verification fluid. In general, verification fluid with

32、a certified induction period is available from the manufacturer of the apparatus. 6 Apparatus 6.1 Automatically controlled oxidation tester, comprising an oxidation reaction vessel containing: test sample cup capable of being rapidly heated; pressure sensor capable of measuring pressures of 1 kPa up

33、 to 2 000 kPa with a resolution of 1 kPa; temperature sensor with a resolution of 0,1 C; pressure and temperature recording of 1 second. The oxidation reaction vessel shall be fitted with filling and relief valves, meant to release the pressure, and a fan to cool the vessel from test to ambient temp

34、erature. The requirements for the apparatus are described in detail in Annex A. 6.2 Pipette, capable of delivering 5,0 ml 0,1 ml. 6.3 O-ring seals, see A.6. 7 Sampling and sample handling Unless otherwise specified, samples shall be taken as described in EN ISO 3170 or EN ISO 3171 and/or in accordan

35、ce with the requirements of national standards or regulations for the sampling of the product under test. Collect and store samples in an opaque container to minimize exposure to light. 8 Performance check of the apparatus 8.1 Verify the correct operation of the equipment by following the procedure

36、in section 10 using the verification fluid (5.4). 8.2 If the induction period of the verification fluid does not meet specified time, repeat 8.1. If it fails a second time, refer to the manufacturers instructions. 8.3 Pressure and temperature are critical parameters. Proper calibration of the respec

37、tive sensors (see 6.1) is therefore important. Recalibrate the tester at least every 12 months for correct temperature and pressure readings. NOTE In view of general good laboratory practice and harmonization of test methods, calibration as in Annex B is strongly recommended. As the calibration proc

38、edure for a pressure sensor is complicated and difficult to be executed by an untrained lab technician, one may (in most cases sufficiently) rely on the verification fluid. DIN EN 16091:2012-02 EN 16091:2011 (E) 6 9 Preparation of the apparatus 9.1 Remove the previous test portion by means of a pipe

39、tte or similar device. 9.2 Remove the used “O-ring“ seal and discard. NOTE To avoid contamination of the new test, it is necessary to discard the used “O-ring“ seal, because it may be soaked with oxidation products from the previous test. 9.3 Wipe the sample cup, the seal groove and the cover with l

40、int-free cleaning tissue (5.3) soaked with cleaning solvent (5.1) until free of gum or other oxidation residues. 9.4 Allow the test sample cup and cover to dry in air and visually inspect for cleanliness. NOTE Compressed air is generally unsuitable to accelerate the evaporation of solvent because it

41、 can contain traces of oil that may influence the next test. 9.5 Insert a new “O-ring“ seal (6.3). 10 Procedure 10.1 Bring the reaction vessel and the sample to be tested to room temperature. 10.2 Using a pipette (6.2), place 5 ml 0,1ml of the sample into the reaction vessel sample cup. 10.3 Cover t

42、he sample-cup with the screw cap (see A.2) and close the reaction vessel. 10.4 Pre-flush the reaction vessel with oxygen. Introduce oxygen (5.2) into the vessel until a pressure of 700 kPa 5 kPa is attained and stabilized over 20 sec. 10.5 Start the heater with no delay between charging with oxygen

43、and starting the test. 10.6 The test temperature of 140 C 0,5 C shall be reached after 270 s 30 s. 10.7 If, during the initial 5 min of the test, a steady drop in pressure is observed, discontinue the test and discard the test specimen. The leakage rate at 140 C with empty sample cup shall not excee

44、d a value of 2 kPa/h. If the leakage rate shows an increase, check the following components: O-ring for damage or residues of samples, surface of sample cup for damage, and sample cup for sample residues. Contact the manufacturer to resolve leakage problems from other parts of the instrument. 10.8 T

45、he apparatus automatically records the temperature (to the nearest 0,1 C) and pressure (to the nearest 1 kPa) of the oxidation vessel continuously. 10.9 The apparatus terminates the test when the pressure readings show a 10 % drop from the maximum observed pressure (breakpoint) and records the time

46、elapsed from the start of the test to the breakpoint (induction period). An example is given in Annex C. 10.10 The apparatus automatically records the average temperature to the nearest 0,1 C as the temperature of the test. DIN EN 16091:2012-02 EN 16091:2011 (E) 7 NOTE The apparatus will automatical

47、ly switch on the fan to cool the reaction vessel to approximately room temperature. When the apparatus has cooled, the pressure is slowly released, at a rate not exceeding 345 kPa/min. 10.11 When the pressure release has finished, open the apparatus and clean according to Clause 9. 11 Expression of

48、results Report the induction period expressed in min., rounded to the nearest 0,01 min. 12 Precision 12.1 General The precision statements were developed in Round Robin tests performed in 2008 and 2009, in accordance with EN ISO 4259 1. This method was tested for FAME, B0, B5, B7, B10, and B30 samples, the induction period measured