DIN EN ISO 3924-2017 Petroleum products - Determination of boiling range distribution - Gas chromatography method (ISO 3924 2016) German version EN ISO 3924 2016《石油产品 沸点范围分布的测定 气相色.pdf

1、January 2017 English price group 14No 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 75.080!%_+“2605908www.din.deDIN

2、EN ISO 3924Petroleum products Determination of boiling range distribution Gas chromatography method (ISO 3924:2016);English version EN ISO 3924:2016,English translation of DIN EN ISO 3924:2017-01Minerallerzeugnisse Bestimmung des Siedeverlaufs Gaschromatographisches Verfahren (ISO 3924:2016);Englisc

3、he Fassung EN ISO 3924:2016,Englische bersetzung von DIN EN ISO 3924:2017-01Produits ptroliers Dtermination de la rpartition dans lintervalle de distillation Mthode par chromatographie en phase gazeuse (ISO 3924:2016);Version anglaise EN ISO 3924:2016,Traduction anglaise de DIN EN ISO 3924:2017-01Su

4、persedesDIN EN ISO 3924:201006www.beuth.deDocument comprises 31 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.01.17 DIN EN ISO 3924:2017-01 2 A comma is used as the decimal marker. National foreword This document (EN ISO 3924

5、:2016) has been prepared by Technical Committee ISO/TC 28 “Petroleum products and related products of synthetic or biological origin” in collaboration with Technical Committee CEN/TC 19 “Gaseous and liquid fuels, lubricants and related products of petroleum, synthetic and biological origin” (Secreta

6、riat: NEN, Netherlands). The responsible German body involved in its preparation was DIN-Normenausschuss Materialprfung (DIN Standards Committee Materials Testing), Working Committee NA 062-06-42 AA Prfung von flssigen Kraftstoffen und Heizlen of the Fachausschuss Minerall- und Brennstoffnormung. Th

7、e DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 3170 DIN EN ISO 3170 ISO 3171 DIN EN ISO 3171 ISO 3405 DIN EN ISO 3405 ISO 4259 DIN EN ISO 4259 Amendments This standard differs from DIN EN ISO 3924:2010-06 as follows: a) a method for an a

8、ccelerated analysis has been introduced; b) the calculation of the volume percentage recovered has been included in Annex A; c) the standard has been editorially revised. Previous editions DIN EN ISO 3924 2010-06 National Annex NA (informative) Bibliography DIN EN ISO 3170, Petroleum liquids Manual

9、sampling DIN EN ISO 3171, Petroleum liquids Automatic pipeline sampling DIN EN ISO 3405, Petroleum products Determination of distillation characteristics at atmospheric pressure DIN EN ISO 4259, Petroleum products Determination and application of precision data in relation to methods of test EUROPEA

10、N STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 3924 October 2016 ICS 75.080 Supersedes EN ISO 3924:2010English Version Petroleum products - Determination of boiling range distribution - Gas chromatography method(ISO3924:2016) Produits ptroliers - Dtermination de la rpartition dans lintervalle de

11、distillation - Mthode par chromatographie en phase gazeuse (ISO 3924:2016) Minerallerzeugnisse - Bestimmung des Siedeverlaufs -Gaschromatographisches Verfahren (ISO 3924:2016)This European Standard was approved by CEN on 15 July 2016. CEN members are bound to comply with the CEN/CENELEC Internal Reg

12、ulations which stipulate 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 mem

13、ber. 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 member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions.

14、CEN members are the national 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

15、, Portugal, Romania, Slovakia, Slovenia, 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 2016 CEN All rights of exploitation in

16、 any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 3924:2016 EEuropean foreword .31 Scope . 52 Normative references 53 Terms and definitions . 54 Principle 65 Reagents and materials . 66 Apparatus . 87 Sampling . 108 Preparation of apparatus . 109 Calibration . 1

17、39.1 Analysis sequence protocol . 139.2 Baseline compensation analysis . 149.3 Retention time versus boiling point calibration .149.4 Analysis of reference material 1410 Procedure1610.1 Sample preparation . 1610.2 Sample analysis . 1611 Calculation .1712 Expression of results .1713 Precision 1813.1

18、General 1813.2 Repeatability 1813.3 Reproducibility 1814 Test report 19Annex A (informative) Calculation of ISO 3405 equivalent data 20Annex B (informative) Accelerated analysis 23Annex C (informative) Boiling points of non-normal alkane hydrocarbons 25Bibliography .29Contents PageDIN EN ISO 3924:20

19、17-01 EN ISO 3924:2016 (E) 2Foreword . 4European foreword This document (EN ISO 3924:2016) has been prepared by Technical Committee ISO/TC 28 “Petroleum products and related products of synthetic or biological origin” in collaboration with Technical Committee CEN/TC 19 “Gaseous and liquid fuels, lub

20、ricants 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 or by endorsement, at the latest by April 2017, and conflicting nat

21、ional standards shall be withdrawn at the latest by April 2017. 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. This document supersed

22、es EN ISO 3924:2010. 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, Estonia, Finland, Former Yugoslav Republic of M

23、acedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 3924:2016 has been approved by

24、CEN as EN ISO 3924:2016 without any modification. DIN EN ISO 3924:2017-01 EN ISO 3924:2016 (E) 3 ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carr

25、ied out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

26、ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the differen

27、t approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives). Attention is drawn to the possibility that some of the elements of this document may b

28、e the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any patent rights identified during the development of the document will be in the Introduction and/or on the ISO list of patent declarations received (see www.iso.org/patents)

29、. Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO principles

30、in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationISO 3924 was prepared by the European Committee for Standardization (CEN) Technical Committee CEN/TC 19, Gaseous and liquid fuels, lubricants and related products of petroleum, synthetic and biologica

31、l origin, in collaboration with ISO Technical Committee ISO/TC 28, Petroleum products and related products of synthetic or biological origin, in accordance with the Agreement on technical cooperation between ISO and CEN (Vienna Agreement).This fourth edition cancels and replaces the third edition (I

32、SO 3924:2010), which has been technically revised. The third edition had several updates regarding the calculation of ISO 34051equivalent data. Because ISO 3924 is extensively used and referenced in many fuel specifications, a faster analysis procedure was included. Many fuel specifications concerne

33、d demand volume percentage recovered at 250C and 350C but this result was not part of the report of ISO 3924 in the former version as described. This is updated with this edition (see Annex A), for which an assessment has been executed by CEN/TC 19. In addition, several editorial updates have been m

34、ade.This method is originally based on the jointed IP 4063and ASTM D28874methods.DIN EN ISO 3924:2017-01 EN ISO 3924:2016 (E) 4 WARNING The use of this International Standard can involve hazardous materials, operations and equipment. This International Standard does not purport to address all of the

35、 safety problems associated with its use. It is the responsibility of users of this International 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.1 ScopeThis Int

36、ernational Standard specifies a method for the determination of the boiling range distribution of petroleum products. The method is applicable to petroleum products and fractions with a final boiling point of 538 C or lower at atmospheric pressure as determined by this International Standard. This I

37、nternational Standard is not applicable to gasoline samples or gasoline components. The method is limited to products having a boiling range greater than 55 C and having a vapour pressure sufficiently low to permit sampling at ambient temperature.The method has successfully been applied to samples c

38、ontaining fatty acid methyl esters (FAME) up to 10 % (V/ V ).NOTE For the purposes of this International Standard, the terms “% (m/m)” and % (V/ V ) are used to represent the mass fraction (), respectively the volume fraction () of a material.2 Normative referencesThe following documents, in whole o

39、r in part, are normatively referenced in this document 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.ISO 3170, Petroleum liquids Manual sampling

40、ISO 3171, Petroleum liquids Automatic pipeline sampling3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.3.1initial boiling pointIBPtemperature corresponding to the retention time at which a net area count equal to 0,5 % of the total sample area unde

41、r the chromatogram is obtained3.2final boiling pointFBPtemperature corresponding to the retention time at which a net area count equal to 99,5 % of the total sample area under the chromatogram is obtainedDIN EN ISO 3924:2017-01 EN ISO 3924:2016 (E) 5 3.3slice ratenumber of data slices acquired per u

42、nit of time used to integrate the continuous (analogue) chromatographic detector response during an analysisNote 1 to entry: The slice rate is expressed in Hz (for example, slices per second).4 PrincipleA sample is introduced into a gas chromatographic column which separates hydrocarbons in the orde

43、r of increasing boiling point. The column temperature is raised at a reproducible rate and the area under the chromatogram is recorded throughout the analysis. Boiling temperatures are assigned to the time axis from a calibration curve, obtained under the same conditions by running a known mixture o

44、f hydrocarbons covering the boiling range expected in the sample. From these data, the boiling range distribution is obtained.Annex A presents a correlation model for the calculation of physical distillation (see References 1, 5 and 6) equivalent data from boiling range distribution analysis by gas

45、chromatography determined following this International Standard.Annex B describes an alternative, accelerated analysis (see 8.2).5 Reagents and materials5.1 Stationary phase for columns, non-polar, that elutes hydrocarbons in boiling point order.NOTE The following materials have been used successful

46、ly as liquid phases.For packed columns: silicone gum rubber UC-W98; silicone gum rubber GE-SE-30; silicone gum rubber OV-1; silicone gum rubber OV-101;For capillary columns: polydimethylsiloxane.5.2 Solid support for packed columns, usually consisting of crushed fire brick or chromatographic diatoma

47、ceous earth.The particle size and support loading shall be such as to give optimum resolution and analysis time.NOTE In general, support loadings of 3 % to 10 % have been found most satisfactory.5.3 Carrier gas, with a minimum purity of 99,995 %, constituted ofa) helium or hydrogen for use with ther

48、mal conductivity detectors, orb) nitrogen, helium, hydrogen or argon for use with flame ionization detectors.5.4 Hydrogen, grade suitable for flame ionization detectors.5.5 Compressed air, free of oil and water, regulated for flame ionization detectors.DIN EN ISO 3924:2017-01 EN ISO 3924:2016 (E) 6 5.6 Calibration mixture, consisting of an accurately weighed mixture of n-alkanes covering the range from C5to C44and dissolve