DIN EN ISO 10370-2015 Petroleum products - Determination of carbon residue - Micro method (ISO 10370 2014) German version EN ISO 10370 2014《石油产品 碳渣的测定 显微法 (ISO 10370-2014) 德文版本 EN .pdf

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1、March 2015 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).ICS

2、75.080!%AQ“2304699www.din.deDDIN EN ISO 10370Petroleum products Determination of carbon residue Micro method (ISO 10370:2014);English version EN ISO 10370:2014,English translation of DIN EN ISO 10370:2015-03Minerallerzeugnisse Bestimmung des Koksrckstandes Mikroverfahren (ISO 10370:2014);Englische F

3、assung EN ISO 10370:2014,Englische bersetzung von DIN EN ISO 10370:2015-03Produits ptroliers Dtermination du rsidu de carbone Mthode micro (ISO 10370:2014);Version anglaise EN ISO 10370:2014,Traduction anglaise de DIN EN ISO 10370:2015-03SupersedesDIN EN ISO 10370:1995-11www.beuth.deDocument compris

4、es 15 pagesIn case of doubt, the German-language original shall be considered authoritative.03.15 DIN EN ISO 10370:2015-03 2 A comma is used as the decimal marker. National foreword This document (EN ISO 10370:2014) has been prepared by Technical Committee ISO/TC 28 Petroleum products and lubricants

5、“ in collaboration with 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 DIN-Normenausschuss Materialprfung(DIN Stand

6、ards Committee Materials Testing), Working Committee NA 062-06-42 AA Prfung von flssigen Kraftstoffen und Heizlen of the Fachausschuss Minerall- und Brennstoffnormung. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. DIN and/or DKE

7、 shall not be held responsible for identifying any or all such patent rights. This second edition cancels and replaces the first edition (ISO 10370:1993), of which it constitutes a minor revision. It also incorporates ISO 10370:1993/Cor1:1996. The DIN Standard corresponding to the International Stan

8、dard referred to in this document is as follows: ISO 3405 DIN EN ISO 3405 Amendments This standard differs from DIN EN ISO 10370:1995-11 as follows: a) normative references have been updated; b) different vial lengths are now given in Figure 2 Sample vial (soda lime glass, bottom) and vial holder (t

9、op); c) the standard has been editorially revised. Previous editions DIN EN ISO 10370: 1995-11 National Annex NA (informative) Bibliography DIN EN ISO 3405, Petroleum products Determination of carbon residue by the micro method EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 10370 November

10、2014 ICS 75.080 Supersedes EN ISO 10370:1995English Version Petroleum products - Determination of carbon residue - Micro method (ISO 10370:2014) Produits ptroliers - Dtermination du rsidu de carbone - Mthode micro (ISO 10370:2014) Minerallerzeugnisse - Bestimmung des Koksrckstandes -Mikroverfahren (

11、ISO 10370:2014) This European Standard was approved by CEN on 9 August 2014. 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 bibli

12、ographical references 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 respons

13、ibility 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 national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Repub

14、lic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMAL

15、ISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2014 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 10370:2014 EContents PageForeword 31 Scope . 42 Normative references 4

16、3 Terms and definitions . 44 Principle 55 Reagents and materials . 56 Apparatus . 57 Sample preparation . 77.1 General instructions . 77.2 Regular procedure . 87.3 Modified procedure 88 Sample transfer . 89 Test procedure 910 Calculation 911 Expression of results . 1012 Precision 1012.1 General 1012

17、.2 Repeatability, r 10112.3 Reproducibility, R 1013 Test report 11Annex A (informative) Relationship of carbon residue (micro method) to carbon residue (Conradson method) . 12Bibliography .13DIN EN ISO 10370:2015-03 EN ISO 10370:2014 (E) 2 Foreword This document (EN ISO 10370:2014) has been prepared

18、 by Technical Committee ISO/TC 28 “Petroleum products and lubricants” in collaboration with 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

19、 a national standard, either by publication of an identical text or by endorsement, at the latest by May 2015, and conflicting national standards shall be withdrawn at the latest by May 2015. Attention is drawn to the possibility that some of the elements of this document may be the subject of paten

20、t rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes EN ISO 10370:1995. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this Europea

21、n 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, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Sloven

22、ia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 10370:2014 has been approved by CEN as EN ISO 10370:2014 without any modification. DIN EN ISO 10370:2015-03 EN ISO 10370:2014 (E) 3 1 ScopeThis International Standard specifies a method for the determin

23、ation of the amount of carbon residue, in the range 0,10 % (m/m) to 30,0 % (m/m), left after evaporation and pyrolysis of petroleum products under specified conditions.NOTE 1 The carbon residue value serves as an approximation of the tendency of petroleum products to form carbonaceous deposits under

24、 similar degradation conditions, and may be useful in the assessment of relative carbon-forming tendencies of products within the same class. In this case, care should be taken in the interpretation of results.For products which yield a residue in excess of 0,10 % (m/m), the test results are equival

25、ent to those obtained by the Conradson carbon residue test (see ISO 66151) in the range of 0,10 (m/m) to 25,0 (m/m) (for details see Annex A).This International Standard is also applicable to petroleum products which consist essentially of distillate material, and which may yield a carbon residue be

26、low 0,10 % (m/m). On such materials, a 10 % (V/ V ) distillation residue is prepared by the procedure described in 7.3.1 and 7.3.2 before analysis.Both ash-forming constituents, as defined by ISO 62452and non-volatile additives present in the sample add to the carbon residue value and are included i

27、n the total value reported.NOTE 2 The presence of organic nitrates incorporated in certain distillate fuels will yield abnormally high values for the carbon residue. The presence of alkyl nitrate in the fuel may be detected by ISO 13759.32 Normative referencesThe following documents, in whole or in

28、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 3405, Petroleum products Determination of di

29、stillation characteristics3 Terms and definitionsFor the purposes of this document, the following term and definition apply3.1carbon residuethe whole residue produced of a sample from the specific conditions of evaporation and pyrolysis described in this International StandardDIN EN ISO 10370:2015-0

30、3 EN ISO 10370:2014 (E) 4WARNING The use of this International Standard may involve hazardous materials, operations, and equipment. This International Standard does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this International S

31、tandard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.4 PrincipleA weighed aliquot of the oil sample is placed in a glass vial and heated to 500 C under an inert (nitrogen) gas stream in a controlled manner for a specific

32、time. Volatiles formed during the reactions are swept away by the inert gas. The carbonaceous residue remaining is weighed.5 Reagents and materials5.1 Nitrogen, low oxygen content, i.e. 99,998 % (V/V) or better, with appropriate regulation to provide a delivery pressure of 0 kPa to 200 kPa.NOTE The

33、practical minimum delivery pressure is 140 kPa.6 Apparatus6.1 Glass sample vials, of 2 ml capacity, 12 mm outside diameter, approximately 35 mm high.A vial of 4 ml capacity, 12 mm outside diameter, approximately 72 mm high may be used with samples of very low carbon residue content, i.e. below appro

34、ximately 0,20 % (m/m), but no precision data has been obtained for them.NOTE 1 An interlaboratory study4has been carried out by the Energy Institute on the 10 % volume distillation residue procedure for middle distillates using 4 ml vials and automatic distillation units and the precision is given i

35、n Clause 12.NOTE 2 A glass sample vial of approximately 20 ml capacity (20,5 mm to 21 mm outside diameter by (701) mm high) for samples that are expected to yield residues 5,0 0,15 0,05Brown or black opaque and mobile 1,0 to 5,0 0,50 0,10Transparent or translucent 0,2 to 1,0 1,50 0,50Middle distilla

36、te, 10 % (V/ V ) residue 0,3 3,00 0,50 when used in conjunc-tion with the 4 ml vialDIN EN ISO 10370:2015-03 EN ISO 10370:2014 (E) 8 9 Test procedure9.1 With the oven at a temperature 100 C, place the vial holder, loaded as in 8.3, into the oven chamber and secure lid. Purge with nitrogen for at leas

37、t 10 min at 600 ml/min. Subsequently, decrease the purge to 150 ml/min and heat the oven slowly to 500 C at a rate of 10 C/min to 15 C/min.9.2 Hold the oven at 500 C 2 C for 15 min. Then shut off furnace power and allow the oven to cool freely while under a nitrogen purge of 600 ml/min. When the ove

38、n temperature is 250 C, remove the vial holder for further cooling in the desiccator.NOTE 1 After the samples are removed from the oven, the nitrogen purge may be shut off.If the sample foams or spatters causing loss of sample, discard and repeat the test.NOTE 2 Spattering may be due to water that m

39、ay be re-moved by prior gentle heating under reduced pressure, followed by a nitrogen sweep. Alternatively, a smaller size may be used.If another test is to be run, remove the lid to allow faster cooling.NOTE 3 A subsequent test may be started when the oven has cooled to below 100 C.WARNING Do not o

40、pen the oven to air at any time during the heating cycle, as the introduction of air (oxygen) may form an explosive mixture with the volatile coking products formed. Do not open the oven until the oven temperature has fallen to below 250 C during the cooling step. Maintain the nitrogen flow until af

41、ter the vial holder has been removed from the oven.Either locate the coking oven in a laboratory exhaust hood for safe venting of smoke and fumes, or install a vent line from the oven exhaust to the laboratory exhaust system, being careful not to create negative pressure in the line.9.3 Handling the

42、 vials with forceps, transfer them to the desiccator and allow them to cool to room temperature.Weigh each cooled vial to the nearest 0,1 mg and record its mass.Discard the used glass sample vials.9.4 Examine the condensate trap at the bottom of the oven chamber; empty if necessary and replace.WARNI

43、NG The condensate trap residue may contain some carcinogenic materials, and contact with them should be avoided. They should be properly disposed of according to acceptable procedures.10 CalculationCalculate the mass percentage of carbon residue in the original sample, or in the 10 % (V/ V ) distill

44、ation residue, to the nearest 0,01 % (m/m), CR, using the following formula:CR=mmmm3121100 (1)wherem1is the mass of the empty vial, in grams;m2is the mass of vial + test portion, in grams;m3is the mass of vial + residue, in grams.DIN EN ISO 10370:2015-03 EN ISO 10370:2014 (E) 9 For the relationship

45、of carbon residue by micro method (this International Standard) to carbon residue by Conradson method (see ISO 66151), Annex A may be used.11 Expression of resultsReport results obtained from Formula (1) as “Carbon residue micro method” to the nearest 0,01 % (m/m).Or report carbon residue micro meth

46、od on 10 % (V/ V ) residue to the nearest 0,01 % (m/m).12 Precision12.1 GeneralThe precision given was derived from statistical analysis by ISO 42595of the results of interlaboratory testing of a matrix of fuels and were first published in 1983. The precision is shown graphically in Figure 3.The pre

47、cision data for 10 % volume residue come from statistical examination of the results of interlaboratory testing according to ISO 4259 of a matrix of fuels including automotive diesel fuels, gasoils, fuels containing up to 10 % (V/ V ) of fatty acid methyl esters (FAME), fuels with cetane improver and marine fuel, which was carried out by the Energy Institute in 2007.12.2 Repeatability, rThe difference between two test results obtained by the same operator with the same ap