EN 17057-2018 en Automotive fuels and fat and oil derivates - Determination of saturated monoglycerides content in Fatty Acid Methyl Esters (FAME) - Method by GC-FID.pdf

1、BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06Automotive fuels and fat and oil derivates - Determination of saturated monoglycerides content in Fatty Acid Methyl Esters (FAME) - Method by GC-FIDBS EN 17057:2018National forewordThis British Standard is the UK implem

2、entation of EN 17057:2018.The UK participation in its preparation was entrusted to Technical Committee PTI/13, Petroleum Testing and Terminology.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the nece

3、ssary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2018 Published by BSI Standards Limited 2018ISBN 978 0 580 95402 3ICS 75.160.20Compliance with a British Standard cannot confer immunity from legal obligations. This British Standard

4、was published under the authority of the Standards Policy and Strategy Committee on 31 March 2018.Amendments/corrigenda issued since publicationDate Text affectedBRITISH STANDARDBS EN 17057:2018EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 17057January 2018ICS 75.160.20EUROPEAN COMMITTEE FOR STA

5、NDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGCEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2018 CEN Ref. No. EN 17057:2018: EAll rights of exploitation in any form and by any means reserved worldwide for CEN national MembersAutomotive fuels and fat and o

6、il derivates - Determination of saturated monoglycerides content in Fatty Acid Methyl Esters (FAME) - Method by GC-FIDCarburants pour automobiles et produits drivs des corps gras - Dtermination de la teneur en monoglycrides saturs (SMG) des esters mthyliques dacides gras (EMAG) - Mthode par GC-FIDKr

7、aftstoffe und Erzeugnisse aus Fetten und len - Bestimmung des Gehalts an gesttigten Monoglyceriden in Fettsure-Methylester (FAME) - Verfahren mit GC-FIDThis European Standard was approved by CEN on 19 November 2017.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipu

8、late the conditions 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 St

9、andard exists 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 na

10、tional standards 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, S

11、erbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom.English VersionEN 17057:2018 (E)European forewordThis document (EN 17057:2018) has been prepared by Technical Committee CEN/TC 19 “Gaseous and liquid fuels, lubricants and related products of petroleum, synthetic and bi

12、ological 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 or by endorsement, at the latest by July 2018 and conflicting national standards shall be withdrawn at the latest by July 2018

13、.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 identifying any or all such patent rights.According to the CEN-CENELEC Internal Regulations, the national standards organization

14、s 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, Lithuania, Luxembourg, Malta,

15、Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.2BS EN 17057:2018EN 17057:2018 (E)European foreword 2European foreword 41 Scope . 52 Normative references 53 Principle 54 Reagents and materials . 55 Apparatus . 65.2

16、.1 DB 5HT (5 % phenyl, 95 % methylpolysiloxane), 30 m x 0,25 mm, 0,1 m film thickness 65.2.2 CP9078, 15 m x 0,32 mm, 0,1 m film thickness. 66 Preparation of solutions . 66.1 Glyceryl monononadecanoate stock solution, 2,5 mg/ml 66.2 Reference solution . 77 Sampling 78 Procedure. 78.1 Operating condit

17、ions . 78.2 Column evaluation . 78.3 Analysis of the reference solution 88.4 Preparation and analysis of the samples 88.5 Identification 98.6 Calibration 99 Determination of results 99.1 Integration of the peaks 99.2 Calculation 910 Expression of results .1011 Precision 1011.1 General 1011.2 Repeata

18、bility, r . 1011.3 Reproducibility, R . 1012 Test report 11Annex A (informative) Saturated monoglyceride standards 12Annex B (informative) Calculation of column performance .13Annex C (informative) Example chromatograms 15Bibliography .163Contents PageBS EN 17057:2018EN 17057:2018 (E)European forewo

19、rdThis document (EN 17057:2018) 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 standar

20、d, either by publication of an identical text or by endorsement, at the latest by July 2018 and conflicting national standards shall be withdrawn at the latest by July 2018.Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/o

21、r CENELEC shall not 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 R

22、epublic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Ki

23、ngdom.4BS EN 17057:2018EN 17057:2018 (E)1 ScopeThis document specifies a method to determine the saturated monoglyceride content in Fatty Acid Methyl Esters (FAME). This method only identifies and quantifies the following saturated monoglycerides: 1-C16:0, 2-C16:0 and 1-C18:0. The total saturated mo

24、noglyceride content is calculated by the summation of the contents of these three saturated monoglycerides. The precision has been established for FAMEs having saturated monoglycerides in the (200 to 1 500) mg/kg range.This method is not suitable for FAME produced from or containing coconut and palm

25、 kernel oil derivatives because of overlapping of various peaks.NOTE This Standard determines only three saturated monoglycerides, i.e. 1-C16:0, 2-C16:0 and 1-C18:0. FAMEs can contain also other saturated monoglycerides such as 1-C17:0, but these are generally much lower than the three targeted satu

26、rated monoglycerides and are therefore not included in the Standards scope.WARNING The use of this standard can 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 responsibility of the user of

27、 this standard to take appropriate measures to ensure the safety and health of personnel prior to application of the standard, and fulfil statutory and regulatory requirements for this purpose.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this docu

28、ment and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.EN ISO 3170, Petroleum liquids Manual sampling (ISO 3170)EN ISO 3171, Petroleum liquids Autom

29、atic pipeline sampling (ISO 3171)3 PrincipleThe saturated monoglycerides are converted into more stable and volatile silyl derivatives in the presence of pyridine and N-methyl-N-trimethylsilyltrifluoroacetamide (MSTFA).After silylation, the sample is analysed by gas chromatography on a capillary col

30、umn with thin film thickness, an on-column injector or equivalent device (e.g. programmed-temperature vaporizing injector), and a flame ionization detector.The quantification of the saturated monoglycerides is performed against the internal standard (IS) Glyceryl monononadecanoate (mono C19), using

31、a relative response factor of 1,00.4 Reagents and materialsUse only reagents of recognized analytical grade. The reagents should not contain components that chromatographically co-elute with the target components, i.e. 1-C16:0, 2-C16:0 and 1-C18:0.NOTE Annex A shows a list of suppliers for saturated

32、 monoglyceride standards.4.1 N-methyl-N-trimethysilyltrifluoroacetamide (MSTFA) CAS: 24589-78-4, p.a.4.2 Pyridine, CAS: 110-86-1, max. 0,1 % water, stored on molecular sieve.4.3 n-Heptane, CAS: 142-82-5, p.a.4.4 2-Hexadecanoyl-glycerol ( ), CAS: 23470-00-0, of 99,0 % purity.5BS EN 17057:2018EN 17057

33、:2018 (E)4.5 1-Hexadecanoyl-rac-glycerol ( ), CAS: 542-44-9, of 99,0 % purity.4.6 1-Octadecanoyl-rac-glycerol ( ), CAS: 123-94-4, of 99,0 % purity.4.7 1-Nonadecanoyl-rac-glycerol ( ), CAS: 112340-30-4, of 99,0 % purity.4.8 Squalene CAS: 111-02-4 (6E,10E,14E,18E)-2,6,10,15,19,23-Hexamethyltetracosa-2

34、,6,10,14,18,22-hexaene), of 99,0 % purity.4.9 n-Hexacosane CAS: 630-01-3 (n-C26), of 99,0 % purity.4.10 n-Octacosane CAS: 630-02-4 (n-C28), of 99,0 % purity.4.11 Carrier gas, hydrogen or helium, minimum 99,999 % purity.4.12 Auxiliary gases, such as air, hydrogen and nitrogen, minimum 99,995 % purity

35、.5 ApparatusUsual laboratory apparatus and glassware, together with the following:5.1 Gas chromatograph, equipped with an on-column injector or equivalent device (e.g. PTV: Programmed Temperature Vaporisor), a temperature programmable oven and a flame ionization detector.5.2 Capillary column, capabl

36、e of being programmed up to 400 C (“high temperature” type), e.g. 5.2.1 or 5.2.2. Other columns with similar performance may be used. Such columns should be tested first before being selected as co-elution may occur.5.2.1 DB 5HT (5 % phenyl, 95 % methylpolysiloxane), 30 m x 0,25 mm, 0,1 m film thick

37、ness.5.2.2 CP9078, 15 m x 0,32 mm, 0,1 m film thickness.5.3 Volumetric flasks, 10, 20 and 50 ml capacity.5.4 Screw-cap vials with PTFE-faced septa, 10 ml capacity.5.5 Precision pipette, 1 ml capacity.5.6 Microsyringes, 100 l and 500 l capacity.5.7 Graduated cylinder, 10 ml capacity.5.8 Analytical ba

38、lance, with an accuracy of 0,1 mg.6 Preparation of solutions6.1 Glyceryl monononadecanoate stock solution, 2,5 mg/mlAccurately weigh approximately 50 mg (accuracy 0,1 mg) of glyceryl monononadecanoate (1-C19:0, 4.7) in a 20 ml volumetric flask (5.3) and make up to the mark with pyridine (4.2).6 BS E

39、N 17057:2018EN 17057:2018 (E)The solution shall be perfectly clear at ambient temperature. After storage in refrigerator at 4 C the solution might show a precipitate that shall spontaneously re-dissolve when put at ambient temperature, without any external heating.NOTE If stored at 4 C the solution

40、is stable for at least 3 months.6.2 Reference solutionPrepare a stock solution of 1-C16:0 (4.5), 2-C16:0 (4.4), 1-C18:0 (4.6), squalene (4.8), n-C26 (4.9) and n-C28 (4.10) by weighing approximately 50 mg (accuracy 0,1 mg) of each in a 50 ml volumetric flask (5.3), dissolve and make up to the mark wi

41、th pyridine (4.2).7 SamplingUnless otherwise specified in the commodity specification, samples shall be taken as described in EN ISO 3170 or EN ISO 3171 and/or in accordance with the requirements of national regulations for the sampling of the product under test.8 Procedure8.1 Operating conditionsTh

42、e chromatographic analysis conditions shall be chosen taking into account the characteristics of the column being used and the type of carrier gas (hydrogen or helium). It is however recommended to observe an analysis time of about 30 min to 35 min. Ensure that the triglycerides are fully eluted to

43、prevent heavy ends built up in the column.By way of indication, an example of analysis conditions is described in Table 1.Table 1 Exemplary analysis conditionsColumn temperature program for column:DB 5HT (5 % phenyl, 95 % methylpolysiloxane), 30 m x 0,25 mm, 0,1 m film thickness60 C hold for 1 min;6

44、0 C to 200 C at 20 C/min;200 C to 250 C at 2 C/min;250 C to 370 C at 20 C/min;370 C hold for 10 minColumn temperature program for column:CP9078, 15 m x 0,32 mm, 0,1 m film thickness60 C hold for 1 min;60 C to 230 C at 20 C/min;230 C to 370 C at 10 C/min;370 C hold for 10 minDetector temperature: 375

45、 CCarrier gasHydrogen or Helium1,5 ml/min (to be optimized for the applied gas type)Injectionmode:volume injected:On-column or PTV1 l8.2 Column evaluationIn order to establish that a column will perform as required, the following specifications shall be determined for new column acceptability and ar

46、e useful for periodic column evaluation.7BS EN 17057:2018EN 17057:2018 (E)During robustness studies, n-C26, n-C28 and squalene were identified as components that can chromatographically co-elute with the target components 1-C16:0 and 1-C18:0. Therefore, resolution requirements are specified for thes

47、e components in Table 2.Table 2 Resolution requirementsPair Required resolution for this pairn-C26 and 1-C16:0 1,0Squalene and 1-C18:0 1,0n-C28 and 1-C18:0 1,0NOTE Meeting these requirements, it is still possible that co-eluting of other components with the target components, i.e. 1-C16:0, 2-C16:0 a

48、nd 1-C18:0 occurs. In that case, the calculated saturated monoglyceride content will be somewhat overestimated. The column temperature programming profile is dependent upon the individual column characteristics. The temperature profile is to be optimized in order to establish satisfactory separation

49、s for the sets of components listed in 6.2.Analyse the reference solution as described in 8.3.The resolution, R, is calculated using the following formula:(1)whereis the retention time of peak 2;is the retention time of peak 1;is the peak width at half height of the first peak;is the peak width at half height of the second peak.Ensure that values for retention time and peak width are in the same units.NOTE Annex B shows an example for the calculation of the resolution.8.3 Analysis of the refe