DIN EN 14108-2015 Fat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of sodium content by atomic absorption spectrometry German version EN 14108 2003《脂肪和油的衍生.pdf

1、June 2015Translation by DIN-Sprachendienst.English price group 8No 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).ICS 67.

2、200.10!%C-N“2321043www.din.deDDIN EN 14108Fat and oil derivatives Fatty Acid Methyl Esters (FAME) Determination of sodium content by atomic absorption spectrometry;English version EN 14108:2003,English translation of DIN EN 14108:2015-06Erzeugnisse aus pflanzlichen und tierischen Fetten und len Fett

3、sure-Methylester (FAME) Bestimmung des Natriumgehaltes durch Atomabsorptionsspektrometrie;Englische Fassung EN 14108:2003,Englische bersetzung von DIN EN 14108:2015-06Produits drivs des corps gras Esters mthyliques dacides gras (EMAG) Dtermination de la teneur en sodium par spectromtrie dabsorption

4、atomique;Version anglaise EN 14108:2003,Traduction anglaise de DIN EN 14108:2015-06SupersedesDIN EN 14108:2003-10www.beuth.deIn case of doubt, the German-language original shall be considered authoritative.Document comprises 11 pages05.15 DIN EN 14108:2015-06 2 A comma is used as the decimal marker.

5、 National foreword This document (EN 14108:2015) has been prepared by Technical Committee CEN/TC 307 “Oilseeds, vegetable and animal fats and oils and their by-products Methods of sampling and analysis” (Secretariat: AFNOR, France) in collaboration with Technical Committee CEN/TC 19 “Gaseous and liq

6、uid fuels, lubricants and related products of petroleum, synthetic and biological origin” (Secretariat: NEN, Netherlands). 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 identi

7、fying any or all such patent rights. The responsible German body involved in its preparation was the DIN-Normenausschuss Materialprfung (DIN Standards Committee Materials Testing), Working Committee NA 062-06-32-01 UA Prfung von FAME of the Fachausschuss Minerall- und Brennstoffnormung in collaborat

8、ion with the DIN-Normenausschuss Lebensmittel und landwirtschaftliche Produkte (DIN Standards Committee Food and Agricultural Products), Working Committee NA 057-05-05 AA Gemeinschaftsausschuss von DIN und DGF fr die Analytik von Fetten, len, Fettprodukten, verwandten Stoffen und Rohstoffen (GA Fett

9、). Amendments Compared with DIN EN 14108:2003-10, the following corrections have been made: a) an information regarding the patent rights has been added to the National foreword; b) a Table of contents has been added; c) in the German version Clause 2 “Prinzip” has been renamed “Kurzbeschreibung“; d

10、) Equation (1) in Clause 6 is no longer numbered; e) in Table A.1 the unit (mg/g) has been replaced by (mg/kg) . Previous editions DIN EN 14108: 2003-10 EN 14108April 2003ICS 67.200.10English versionFat and oil derivatives - Fatty Acid Methyl Esters (FAME) -Determination of sodium content by atomic

11、absorptionspectrometryProduits drivs des corps gras - Esters mthyliquesdacides gras (EMAG) - Dtermination de la teneur ensodium par spectromtrie dabsorption atomiqueErzeugnisse aus pflanzlichen und tierischen Fetten undlen - Fettsure-Methylester (FAME) - Bestimmung desNatriumgehaltes durch Atomabsor

12、ptionsspektrometrieThis European Standard was approved by CEN on 2 January 2003.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bib

13、liographical references concerning such nationalstandards may be obtained on application to the 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 translationunder the responsibility of a

14、CEN member into its own language and notified to the Management Centre has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherl

15、ands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland and United Kingdom.Management Centre: rue de Stassart, 36 B-1050 Brussels 2003 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 14108:2003 EEUROPEAN STANDARDNORME EUROPENNEE

16、UROPISCHE NORMEUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGEN 14108:2003 (E)2ForewordThis document (EN 14108:2003) has been prepared by Technical Committee CEN/TC 307 “Oilseeds, vegetableand animal fats and oils and their by-products - Methods of

17、sampling and analysis“, the secretariat of which is heldby AFNOR.This European Standard shall be given the status of a national standard, either by publication of an identical text orby endorsement, at the latest by October 2003 and conflicting national standards shall be withdrawn at the latest byO

18、ctober 2003.This document has been prepared under Mandate M/245 on Fatty Acid Methylester (FAME) given to CEN by theEuropean Commission and the European Free Trade Association, and supports essential requirements of EUDirective(s).Annex A is informative.According to the CEN/CENELEC Internal Regulati

19、ons, the national standards organizations of the followingcountries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal,Slovakia, Spain, Sweden, S

20、witzerland and the United Kingdom.DIN EN 14108:2015-06EN 14108:2003 (E)31 ScopeThis European standard specifies a method for the determination of sodium contents equal to or greater than1 mg/kg.This method is applicable to fatty acid methyl esters intended for addition to mineral oils.WARNING The us

21、e of this method may involve hazardous equipment, materials and operations. Thismethod does not purport to address to all of the safety problems associated with its use, but it is theresponsibility of the user to search and establish appropriate safety and health practices and determinethe applicabi

22、lity of regulatory limitations prior to use.2 PrincipleThe vegetable oil methyl ester sample is diluted with a xylene solution.The sodium content in the sample is directly determined by flame atomic absorption spectrometry at thewavelength of 589 nm. The calibration solutions used are prepared from

23、a sodium organometallic salt dissolved ina mixture of xylene and stock oil. The addition of stock oil to the calibration solutions is necessary in order toimprove their storage (the low element contents are unstable) and the linearity of the calibration.WARNING The ester sample shall be diluted at l

24、east 25 times with xylene so that the comparison of themeasurements of the sample solution and standards is valid.NOTE Xylene can be replaced by cyclohexane or light petroleum in those laboratories that are not authorized to usearomatic solvents.3 ReagentsUse only reagents of recognised analytical g

25、rade, unless otherwise specified.3.1 Recommendations for washing glasswareThe glassware used for the preparation of the solutions shall be washed at least twice with an approximate 5 mol/lsolution of hydrochloric acid, rinsed with distilled water then dried in order to avoid sodium pollution.3.2 Xyl

26、ene (mixture of isomers)WARNING Inflammable and noxious.3.3 Stock oil 75 (75 mm2/s)1)3.4 Stock oil solution in xylene (200 g/l); dilute in a 200 ml volumetric flask, 40 g of stock oil (3.3) with xylene.Store this solution in a polypropylene bottle.3.5 Sodium, solution in oil (5 000 mg/kg)1). Ready-t

27、o-use solution of a sodium organometallic salt in stock oil,having a certified titre.3.6 Sodium, solutions of intermediary dilutions for the preparation of the set of calibration solutions.1) Products available commercially from CONOSTAN Standard, supplied by Conostan Division, Continental Oil Co, P

28、oncaCity, OK 74601 USA.SPEX Standard supplied by SPEX Industries, Inc. Chemical Sales Department, 3880 Park Avenue, Edison, NJ 08820 - USA.This information is given for the convenience of users of this European Standard and does not constitute an endorsement byCEN of these products.DIN EN 14108:2015

29、-06EN 14108:2003 (E)43.6.1 Sodium, solution in xylene (500 mg/l): weigh, to within 0,001 g, approximately 2,5 g of the sodium solution(3.5) in a 25 ml volumetric flask and dilute to the mark with xylene.This solution may be stored for a month.3.6.2 Sodium, solution in xylene (5 mg/l): sample, using

30、a pipette, 0,50 ml of the sodium standard solution(3.6.1), transfer into a 50 ml volumetric flask and dilute to the mark with xylene.Prepare a new solution each day.NOTE The solutions of intermediary dilutions may be prepared in glass flasks (the sodium pollution being negligible atthese contents).4

31、 Apparatus4.1 Atomic absorption spectrometerAny atomic absorption spectrometer may be used provided that it is equipped with:4.1.1 A hollow sodium cathode lamp.4.1.2 A nebulization system suited for the organic solutions, of which the materials are solvent-resistant.4.1.3 A burner head capable of be

32、ing used with organic solutions and an air-acetylene flame.4.2 Balance, with an accuracy of 1 mg.4.3 Glassware4.3.1 25 ml and 50 ml volumetric flasks.4.3.2 0,5 ml graduated precision pipette.4.4 Polypropylene ware4.4.1 50 ml and 200 ml volumetric flasks.4.4.2 10 ml pipette.4.4.3 250 ml bottles4.4.4

33、Automatic pipette having a variable volume of 1 ml to 5 ml, fitted with ejectable and disposablepolypropylene tips.5 ProcedureWARNING In order to avoid polluting the sodium solutions, it is recommended to prepare all thedetermination solutions in polypropylene flasks and to conduct all the sampling

34、operations usingpolypropylene pipettes or pipettes having disposable polypropylene tips. It is however possible to useglassware taking cleaning precautions in order to avoid pollution by the elements being analysed.5.1 SamplingSampling is not part of the method spacified in this European Standard. A

35、 recommended sampling method is givenin EN ISO 5555 1.DIN EN 14108:2015-06EN 14108:2003 (E)55.2 Preparation of the sample5.2.1 Weigh to within 0,001 g approximately 2 g (mass m in g) of ester sample in a 50 ml volumetric flask(volume V in ml) and dilute to the mark with xylene.5.2.2 Sample two test

36、portions per sample.5.3 Preparation of the set of calibration solutions5.3.1 Prepare the calibrations solutions having the following sodium contents:0,1 mg/l - 0,2 mg/l - 0,3 mg/l.5.3.2 Using a variable volume automatic pipette, transfer 1,00 ml, 2,00 ml and 3,00 ml of the 5 mg/l sodiumsolution (3.6

37、.2) into 50 ml volumetric flasks.5.3.3 With a polypropylene pipette, add to each flask 10 ml of the 200 g/l solution of stock oil in xylene (3.4) anddilute to the mark with xylene.5.3.4 Prepare the zero member or blank test in the same manner without adding any sodium solution.5.3.5 Prepare the cali

38、bration solutions just prior to their measurement on account of their instability.5.4 Spectrometric measurements5.4.1 Preparation of the spectrometerSet the wavelength at 589,0 nm and the band pass at 0,5 nm;conduct the aspiration of the 0,3 mg/l calibration solution in order to optimize the differe

39、nt instrument settings.Seek the maximum response of the signal by adjusting:the air-acetylene gaseous mixture;the aspiration speed of the solution;the burner position.conduct the aspiration of the xylene placed in a polypropylene bottle in order to set the instrument at zeroabsorbance.5.4.2 Calibrat

40、ionConduct the aspiration of the blank (or zero member) and calibration solutions and carry out three measurementsfor each of them.Calculate for each solution the arithmetical mean of the three measurements.Plot the calibration curve from the means obtained.By way of indication, the value of the opt

41、ical density obtained for a 0,3 mg/l concentration is approximately 0,290and the curve is more or less a straight line in the range considered.5.4.3 SamplesConduct the aspiration of the solutions of the samples and carry out the measurements in the same way as for thestandards.DIN EN 14108:2015-06EN

42、 14108:2003 (E)6NOTE In the case where the measurement of the sample exceeds the set of calibration solutions given in 5.3, preparestandards having higher sodium contents, the maximum content being 1 mg/l.6 Expression of resultsDetermine the sodium contents c1and c2in mg/l of the two test portions o

43、f the sample, by referring to thecalibration curve.Calculate the sodium contents C1and C2of the sample, expressed in mg/kg, using the equation:mVcC =wherem is the mass (in grams) of the sample test portion;V is the volume of the sample solution (in millilitres).Calculate the mean content C of sodium

44、 in the sample from C1and C2.Express the result in mg/kg, to the nearest 0,1 mg/kg.7 PrecisionAn interlaboratory test organized in 2000 at European level with the participation of 13 laboratories, each havingcarried out two determinations on each sample, gave the statistical results indicated in ann

45、ex A.7.1 RepeatabilityThe absolute difference between two independent single test results, obtained using the same method on identicaltest material in the same laboratory by the same operator using the same equipment within a short time interval,shall not be greater than:r = 0,086 X + 0,242more than

46、 once out of 20 determinations.7.2 ReproducibilityThe absolute difference between two single test results, obtained using the same method on identical test materialin different laboratories by different operators using different equipment, shall not be greater than:R = 0,263 X + 1,355more than once

47、out of 20 determinations.8 Test reportThe test report shall specify:all information necessary for the complete identification of the sample;the sampling method used if known;the test method used, with reference to this European standard;DIN EN 14108:2015-06EN 14108:2003 (E)7all operating details not

48、 specified in this European Standard, or regarded as optional, together with details ofany incidents which may have influenced the test result(s);the test result(s) obtained, or if the repeatability has been checked, the final quoted result obtained.DIN EN 14108:2015-06EN 14108:2003 (E)8Annex A(info

49、rmative)Results of an interlaboratory trialResults of an interlaboratory trial.A European collaborative test involving 13 laboratories in 6 countries was carried out on 5 samples:Sample 1: FAME prepared from rapeseed oil;Sample 2: FAME prepared from sunflower oil;Sample 3: FAME prepared from a mixture of rapeseed and sunflower oils (80:20);Sample 4: FAME prepared from a mixture of rapeseed and sunflower oils (60:40);Sample 5: FAME prepared from rapeseed oil.Th