DIN EN ISO 15351-2010 Steel and iron - Determination of nitrogen content - Thermal conductimetric method after fusion in a current of inert gas (Routine method) (ISO 15351 1999) Ge.pdf

1、August 2010 Translation by DIN-Sprachendienst.English price group 11No 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、 77.080.01!$j6Z“1711955www.din.deDDIN EN ISO 15351Steel and iron Determination of nitrogen content Thermal conductimetric method after fusion in a current of inert gas(Routine method) (ISO 15351:1999)English translation of DIN EN ISO 15351:2010-08Stahl und Eisen Bestimmung des Stickstoffgehaltes Mes

3、sung der Wrmeleitfhigkeit nach Aufschmelzen in strmendem Inertgas(Routineverfahren) (ISO 15351:1999)Englische bersetzung von DIN EN ISO 15351:2010-08Aciers et fontes Dosage de lazote Mthode par conductibilit thermique aprs fusion sous gaz inerte (Mthode pratique)(ISO 15351:1999)Traduction anglaise d

4、e DIN EN ISO 15351:2010-08www.beuth.deIn case of doubt, the German-language original shall be considered authoritative.Document comprises 16 pages07.10 DIN EN ISO 15351:2010-08 2 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee ISO/TC 17

5、 “Steel” and has been taken over by Technical Committee ECISS/TC 102 “Methods of chemical analysis for iron and steel” (Secretariat: SIS, Sweden) as a European Standard without any modification. The responsible German body involved in its preparation was the Normenausschuss Eisen und Stahl (Iron and

6、 Steel Standards Committee), Working Committee NA 021-00-30 AA Analyseverfahren. There is no national standard on the subject. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 385-1 DIN EN ISO 385 (supersedes DIN 12700-1, withdrawn 2005-

7、07) ISO 648 DIN EN ISO 648 ISO 1042 DIN EN ISO 1042 ISO 3696 DIN ISO 3696 ISO 5725-1 DIN ISO 5725-1 ISO 5725-2 DIN ISO 5725-2 ISO 5725-3 DIN ISO 5725-3 ISO 10720 DIN EN ISO 10720 ISO 14284 DIN EN ISO 14284 National Annex NA (informative) Bibliography DIN EN ISO 385, Laboratory glassware Burettes DIN

8、 EN ISO 648, Laboratory glassware Single-volume pipettes DIN EN ISO 1042, Laboratory glassware One-mark volumetric flasks DIN ISO 3696, Water for analytical laboratory use Specification and test methods DIN ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results Part 1: Gene

9、ral principles and definitions DIN ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method DIN ISO 5725-3, Accuracy (trueness and precision) of measurement method

10、s and results Part 3: Intermediate measures of the precision of a standard measurement method DIN EN ISO 10720, Steel and iron Determination of nitrogen content Thermal conductimetric method after fusion in a current of inert gas DIN EN ISO 14284, Steel and iron Sampling and preparation of samples f

11、or the determination of chemical composition EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 15351 April 2010 ICS 77.080.01 English Version Steel and iron - Determination of nitrogen content - Thermal conductimetric method after fusion in a current of inert gas (Routine method) (ISO 15351:1

12、999) Aciers et fontes - Dosage de lazote - Mthode par conductibilit thermique aprs fusion sous gaz inerte (Mthode pratique) (ISO 15351:1999) Stahl und Eisen - Bestimmung des Stickstoffgehaltes - Messung der Wrmeleitfhigkeit nach Aufschmelzen in strmendem Inertgas (Routineverfahren) (ISO 15351:1999)T

13、his European Standard was approved by CEN on 18 March 2010. 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 refere

14、nces concerning such national standards may be obtained on application to the CEN 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 member i

15、nto its own language and notified to the CEN 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, Iceland, Ireland, It

16、aly, 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: Avenue Marnix 17, B-10

17、00 Brussels 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 15351:2010: EContentsDIN EN ISO 15351:2010-08 EN ISO 15351:2010 (E) 2 Foreword3 1 Scope 4 2 Normative references 4 3 Principle5 4 Reagents and materials.5 Apparat

18、us .5 6 Sampling.6 7 Procedure .6 8 Expression of results 8 Annex A (informative) Features of commercial resistive electrode furnaces and nitrogen analysers.10 Annex B (informative) Additional information on the international cooperative tests.12 9 Test report 9 Annex C (informative) Graphical repre

19、sentation of precision data14 PageForewordDIN EN ISO 15351:2010-08 EN ISO 15351:2010 (E) 3 The text of ISO 15351:1999 has been prepared by Technical Committee ISO/TC 17 “Steel” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 15351:2010 by Technical Commi

20、ttee ECISS/TC 102 “Methods of chemical analysis for iron and steel” the secretariat of which is held by SIS. 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 October 2010, and conflicting national

21、standards shall be withdrawn at the latest by October 2010. 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/CENEL

22、EC 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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania

23、, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 15351:1999 has been approved by CEN as a EN ISO 15351:2010 without any modification. 1 ScopeThis International Standard speci

24、fies a thermal conductimetric method after fusion under inert gas for thedetermination of nitrogen in steel and iron.The method is applicable to nitrogen contents between 0,002 % (m/m) and 0,6 % (m/m).2 Normative referencesThe following normative documents contain provisions which, through reference

25、 in this text, constitute provisions ofthis International Standard. For dated references, subsequent amendments to, or revisions of, any of thesepublications do not apply. However, parties to agreements based on this International Standard are encouraged toinvestigate the possibility of applying the

26、 most recent editions of the normative documents indicated below. Forundated references, the latest edition of the normative document referred to applies. Members of ISO and IECmaintain registers of currently valid International Standards.ISO Guide 31:1981, Contents of certificates of reference mate

27、rials.ISO Guide 35:1989, Certification of reference materials General and statistical principles.ISO 385-1:1984, Laboratory glassware Burettes Part 1: General requirements.ISO 648:1977, Laboratory glassware One-mark pipettes.ISO 1042:1998, Laboratory glassware One-mark volumetric flasks.ISO 3696:198

28、7, Water for analytical laboratory use Specification and test methods.ISO 5725-1:1994, Accuracy (trueness and precision) of measurement methods and results Part 1: Generalprinciples and definitions.ISO 5725-2:1994, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic me

29、thodfor the determination of repeatability and reproducibility of a standard measurement method.ISO 5725-3:1994, Accuracy (trueness and precision) of measurement methods and results Part 3: Intermediatemeasures of the precision of a standard measurement method.ISO 10702:1993, Steel and iron Determin

30、ation of nitrogen content Titrimetric method after distillation.ISO 10720:1997, Steel and iron Determination of nitrogen content Thermal conductimetric method afterfusion in a current of inert gas.ISO 14284:1996, Steel and iron Sampling and preparation of samples for the determination of chemicalcom

31、position.DIN EN ISO 15351:2010-08 EN ISO 15351:2010 (E) 4 3PrincipleFusion of a test portion in a single-use graphite crucible under helium gas at a high temperature (e.g. 2 200 Gb0C).Extraction of the nitrogen in the form of molecular nitrogen in the stream of helium.Separation from the other gaseo

32、us extracts and measurement by thermal conductimetric method.Calibration graph established using steel or iron certified reference materials (CRM).NOTE The accuracy of the method is largely dependant upon the accuracy of the method used to certify the nitrogenconcentration of CRMs as well as upon th

33、eir homogeneity. These calibration specimens shall be ECRM, NIST, JK, JSS, CMSIand other national or international CRMs.4 Reagents and materialsDuring the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only grade 3water as specified in ISO 3696.4.1 Water, pre

34、pare just before use.4.2 Helium, high purity, total impurity content 0,000 5 % (m/m).An oxidation reagent or catalyst copper(II) oxide or platinum tube heated to a temperature above 450 Gb0C shall beused prior to a purifying unit, when the presence of organic contaminants is suspected in the helium.

35、4.3 Copper (II) oxide, on granulated support.4.4 Magnesium perchlorate Mg (ClO4)2(commercial designation: anhydrone), particle size: from 1,2 mm to2 mm, or anhydrous calcium sulfate, (commercial designation: drierite), particle size from 0,6 mm to 0,85 mm.4.5 Sodium hydroxide, on granulated support

36、(commercial designation: ascarite), particle size: from 0,7 mm to1,2 mm.4.6 Appropriate solvent, suitable for washing greasy or dirty test samples, e.g. acetone.4.7 Steel or iron reference materials (RM), one or more of whose property values are sufficientlyhomogeneous as described in ISO Guide 35 a

37、nd well-established for use in the calibration of an apparatus, theassessment of a measurement method or for assigning values to materials.4.8 Steel or iron certified reference materials (CRM), steel or iron reference materials (4.7), accompanied bya certificate in accordance with ISO Guide 31 and o

38、ne or more of whose chemical element concentrations havebeen established, in accordance with ISO Guide 35, by a referee method (e.g. ISO 10702 and 10720) whichestablishes its traceability to an accurate realization of the unit in which the property values are expressed, and forwhich each certified v

39、alue is accompanied by an uncertainty at a stated level of confidence.5 ApparatusDuring the analysis, unless otherwise stated, use only ordinary laboratory apparatus.All volumetric glassware shall be class A, in accordance with ISO 385-1, ISO 648 or ISO 1042 as appropriate.The apparatus required for

40、 fusion of the test portion and separation and measurement of the extracted nitrogenmay be obtained commercially from a number of manufacturers. Follow the manufacturers instructions for theoperation of the instrument.Features of commercial instruments are given in annex A.DIN EN ISO 15351:2010-08 E

41、N ISO 15351:2010 (E) 5 5.1 Graphite crucible, single-use.Use high purity crucibles suitable for use with the apparatus.5.2 Crucible tongs, for handling the crucibles used.5.3 Glass-wool filters.6 SamplingCarry out sampling in accordance with ISO 14284 or appropriate national standards for steel and

42、iron.7 ProcedureWARNING The risks involved when using an apparatus for fusing the test portion are mainly risks ofburns. It is therefore essential to use crucible tongs (5.2) and appropriate containers for the crucibles used.7.1 GeneralKeep the glass-wool filters (5.3) clean. Using a certified refer

43、ence material, verify the effectiveness of the installedreagents (4.3, 4.4 and 4.5) and change them if necessary.In certain instruments, it is necessary to clean the sample introduction pipe in the furnace after each analysis inorder to eliminate carbon deposits. If the electricity supply has been s

44、witched off for a long time, allow time for theinstrument to stabilize as recommended by the manufacturer.After changing the filters (5.3) and/or reagents (4.3, 4.4 and 4.5), or when the apparatus has been inoperative for aperiod, stabilize the instrument by carrying out trial analyses, the results

45、of which are to be disregarded, thenproceed with calibration as indicated in 7.5 before analysing the sample.If the instrument used provides a direct reading in percentage of nitrogen, adjust the instrument reading for eachcalibration range as follows.Read the content of a certified reference materi

46、al of high nitrogen content at various power settings. The requiredheating power for the determination of test samples is that at which the reading levels off.In order to determine a high alloy test sample a high alloy certified reference material shall be used to know therequired heating power.7.2

47、Test portionDegrease the test sample by washing in a suitable solvent (4.6). Evaporate the last traces of the washing liquid byheating.Weigh, to the nearest 1 mg, approximately 1 g of the test sample for nitrogen contents up to 0,1 % (m/m)andapproximately 0,5 g for nitrogen contents greater than 0,1

48、 % (m/m).NOTE The mass of the test portion may be dependent on the type of instrument used.7.3 Blank testPrior to the determination, carry out the following blank tests in duplicate.Place a graphite crucible (5.1) in the furnace (see annex A) and then degas by heating at a temperature greaterthan 2

49、200 Gb0C. Operate the furnace in accordance with the manufacturers instructions.DIN EN ISO 15351:2010-08 EN ISO 15351:2010 (E) 6 Obtain the reading of the blank tests and convert it to micrograms of nitrogen by means of the calibration graph(see 7.5).The mean blank value (m1) is calculated from the two blank values.NOTE It is essential that neither the mean blank value nor the difference between the two blank values exceed 10 G6dgofnitrogen. If these values are abnormally high, the source of