DIN EN ISO 4945-2010 Steel - Determination of nitrogen content - Spectrophotometric method (ISO 4945 1977) German version EN ISO 4945 2009《钢 氮含量的测定 分光光度法》.pdf

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1、March 2010 Translation by DIN-Sprachendienst.English price group 9No 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 7

2、7.080.20!$a.“1621125www.din.deDDIN EN ISO 4945Steel Determination of nitrogen content Spectrophotometric method (ISO 4945:1977)English translation of DIN EN ISO 4945:2010-03Stahl Bestimmung des Stickstoffgehalts Spektralphotometrisches Verfahren (ISO 4945:1977)Englische bersetzung von DIN EN ISO 494

3、5:2010-03Acier Dosage de lazote Mthode spectrophotomtrique (ISO 4945:1977)Traduction anglaise de DIN EN ISO 4945:2010-03www.beuth.deIn case of doubt, the German-language original shall be considered authoritative.Document comprises 11 pages03.10 DIN EN ISO 4945:2010-03 2 A comma is used as the decim

4、al marker. National foreword This standard has been prepared by Technical Committee ISO/TC 17 “Steel” in collaboration with Technical Committee ECISS/TC 20 “Methods of chemical analysis of ferrous products” (Secretariat: SIS, Sweden). The responsible German body involved in its preparation was the N

5、ormenausschuss Eisen und Stahl (Steel and Iron Standards Committee), Working Committee 30 Analyseverfahren. A national standard corresponding to International Standard ISO 4945 is not yet available. EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 4945 October 2009 ICS 77.080.20 English Vers

6、ion Steel - Determination of nitrogen content - Spectrophotometric method (ISO 4945:1977) Acier - Dosage de lazote - Mthode spectrophotomtrique (ISO 4945:1977) Stahl - Bestimmung des Stickstoffgehalts - Spektralphotometrisches Verfahren (ISO 4945:1977) This European Standard was approved by CEN on 5

7、 October 2009. 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 references concerning such national standards may b

8、e 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 into its own language and notified to the CEN

9、Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands

10、, 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-1000 Brussels 2009 CEN All rights of exploitation in any

11、 form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 4945:2009: EContents Page Foreword3 1 Scope 4 2 Field of application 4 3 Reference4 4 Principle4 5 Reagents.4 6 Apparatus .5 7 Sampling.7 8 Procedure .5 8.1 Test portion 5 8.2 Blank test5 8.3 Determination.5 8.4 Plot

12、ting of the calibration curve.6 9 Expression of results 7 10 Test report 7 2 EN ISO 4945:2009 (E) DIN EN ISO 4945:2010-03 Foreword The text of ISO 4945:1977 has been prepared by Technical Committee ISO/TC 17 “Steel” of the International Organization for Standardization (ISO) and has been taken over

13、as EN ISO 4945:2009 by Technical Committee ECISS/TC 20 “Methods of chemical analysis of ferrous products” 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 A

14、pril 2010, and conflicting national standards shall be withdrawn at the latest by April 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

15、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, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland,

16、 Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 4945:1977 has been approved by CEN as a EN ISO 4945:2009 without any modification. 3 EN ISO 4945:200

17、9 (E) DIN EN ISO 4945:2010-03 1 SCOPE This International Standard specifies a spectrophotometric method for the determination of the nitrogen content of non-alloy and low-alloy steels. This method allows the determination only of the nitrogen content which tan be converted to an ammonium salt. 2 FIE

18、LD OF APPLICATION The method is applicable to non-alloy and low-alloy steels containing between 0,002 % and 0,050 % (mlm) of nitrogen and less than 0,6 % (mlm) of Silicon. 3 REFERENCE ISOIR 377, Selection and preparation of samples and test pieces for wrough t steei. 4 PRINCIPLE Dissolution of a tes

19、t Portion in dilute sulphuric acid. After concentration, progressive increasing of the tem- perature to above 300 “C. Separation of ammonia from the ammonium salt formed, by displacement and distillation in a boiling sodium hydroxide medium and collecting in an acid medium. At ambient temperature, f

20、ormation of a blue-coloured complex between the ammonium ions and Phenol in the presence of sodium hypochlorite and sodium pentacyano- nitrosyIferrate( II) (sodium nitroprusside). Spectro- photometric measurement of the complex at a wavelength of about 640 nm. 5 REAGENTS During the analysis, use onl

21、y reagents of recognized analytical grade. 5.1 Distilled or de-ionized water, free from nitrogen compounds, purified by a second passage through ion- exchange resins. 5.2 Potassium sulphate, anhydrous (K,SO,). 5.3 Sulphuric acid, p approximately 1,84 g/ml, about 96 % (m/m) Solution, free from nitrog

22、en compounds. 5.4 Sulphuric acid, p approximately 1,21 g/ml, about 29 % (mlm) solution. Add in small portions, whilst cooling, 200 ml of sulphuric acid (5.3) to about 700 ml of water (5.1), make up the volume to 1 000 ml with water (5.1) and mix. 5.5 Sodium hydroxide, approximately 12 N Solution. Di

23、ssolve, with caution, 480 g of sodium hydroxide pellets in 700 ml of water (5.1) contained in a poly- tetrafluoroethylene beaker. Heat the Solution to boiling and boil for 10 min. Cool, make up the volume to 1 000 ml with water (5.1) and mix. Store in a suitable plastics Container. 5.6 Sulphuric aci

24、d, approximately 1 N Solution. Add 30 ml of sulphuric acid (5.3) to about 700 ml of water (5.1); after cooling make up the volume to 1 000 ml with water (5.1) and mix. 5.7 Sulphuric acid, approximately 0,04 N Solution. Dilute 40 ml of sulphuric acid Solution (5.6) to 1 000 ml with water (5.1) and mi

25、x. 5.8 Sodium hydroxide, approximately 0,2 N Solution. Dilute 30 ml of a 250 g/l Solution of sodium hydroxide with water (5.1), make up the volume to 1 000 ml with water (5.1) and mix. 5.9 Sodium phenate Solution. Add, whilst agitating and cooling, 5 g of Phenol to a mixture of 10 ml of a 250 g/l So

26、lution of sodium hydroxide and 80 ml of water (5.1). Make up the volume to 100 ml with water (5.1) and mix. Prepare this Solution at the time of use. 5.10 Disodium hydrogen Phosphate, 0,l M Solution. Dissolve 36 g of disodium hydrogen Phosphate dodeca- hydrate (Na,HP0,.12H,O) in water (5.1), make up

27、 the volume to 1 000 ml with water (5.1) and mix. 5.11 Disodium pentacyanonitrosylferrate( I I ), 0,25 g/l Solution. Dissolve IO g of disodium pentacyanonitrosylferrate( II) 4 EN ISO 4945:2009 (E) DIN EN ISO 4945:2010-03 dihydrate (sodium nitroprusside) Na, Fe (CN), N0.2H,O in water (5.1), make up t

28、he volume to 1 000 ml with watet- (5.1) and mix. 8 PROCEDURE NOTE - Carry out operations in a from all work on nitrogenous products. weil-ventilated room away At the moment of use, dilute 25 ml of this Solution to 1 000 ml with water (5.1). 8.1 Test Portion Weigh, to the nearest 0,001 g, masses of 1

29、 g and 2 g respect- ively of the test Sample, to be treated concurrently. 5.12 Sodium hypochlorite, approximately 0,l N Solution (approximately 0,3 % (mlm) of active chlorine). Store this Solution at a temperature less than 10 “C. 8.2 Blank test The procedure specified in 8.3 and 8.4 eliminates the

30、inci- derice of the value of the blank test when the same reagents are used with the two test portions indicated in 8.1. 5.13 Nitrogen, Standard Solution corresponding to 0,100 0 g of nitrogen (N) per litre. Weigh, to the nearest 0,l mg, 0,471 6 g of dry ammonium sulphate, dissolve in water (5.1) an

31、d transfer the Solution quantitatively to a 1 000 ml one-mark volumetric flask. Dilute to the mark and mix. 8.3 Determination 8.3.1 Prepara tion c3 f the test Solution 1 ml of this Standard Solution contains 100 pg of nitrogen (N). In a 150 ml Kjeldahl flask covered with a watch-glass, dissolve the

32、test Portion (8.1) with 30 ml of sulphuric acid Solution (5.4). Allow to digest, taking care that the temperature of the liquid does not exceed 90 C, until the release of hydrogen has definitely ceased. 5.14 Nitrogen, Standard Solution corresponding to 0,002 0 g of nitrogen (N) per litre. Transfer 2

33、0,O ml of the Standard nitrogen Solution (5.13) to a 1 000 ml one-mark volumetric flask, dilute to the mark with water (5.1) and mix. When the release of hydrogen has ceased, remove the watch-glass and heat until white sulphuric fumes begin to appear. 1 ml of this Standard Solution contains 2 pg of

34、nitrogen (N). Then add - 5 ml of sulphuric acid (5.3) and Prepare this Standard Solution at the time of use. - 1 g of potassium sulphate (5.2). 5.15 Methyl red, 0,l g/l Solution. Heat for 2 h at a temperature above 300 OC, in such a way that the mixture remains liquid. Cool, add IO ml of water (5.1)

35、 and heat to dissolve the majority of the sulphates. Dissolve 0,l g of methyl red in water (5.1), make up the volume to 1 000 ml with water (5.1) and mix. 8.3.2 Distilla tion The distillation additional steam. may be carried out with or without 6 APPARATUS Ordinary laboratory apparatus and NOTE - Th

36、e fl asks used in d istillation are attacked sodium hydroxide Solution; Change them frequently. by the 6.1 Semi-micro apparatus for additional steam (see figure 1) or distillation without 8.3.2. STEA 1 DISTILLATION WITHOUT ADDITIONAL M 6.2 Apparatus for distillation under a current of steam (see fig

37、ure 2). Use the apparatus shown in figure 1 (6.1). To collect the distillate, transfer 5 ml of sulphuric acid Solution (5.6) to a 100 ml volumetric flask with a ground neck and having a mark at 85 ml. Introduce the tapered tube extension of the condenser into the flask in such a manner that it is im

38、mersed in the sulphuric acid Solution (5.6). 6.3 Spectrophotometer. NOTE - All glassware shall be cl eaned Prior to use in hot sulphuric- Chrom ic acid prepared f rom pure ingredients and water (5. 1). Pass the test Solution (8.3.1) quantitatively into the distillation flask, rinsing with 60 ml of w

39、ater (5.1), add 50 ml of sodium hydroxide Solution (5.5) and rinse the neck of the flask with 30 ml of water (5.1). The final volume of the Solution should be approximately 160 to 165 ml. Moisten the ground neck and connect the flask 7 SAMPLING Sampling shall be carried out in accordance with ISO/R

40、377. For wrought steels not complying with lSO/R 377, the appropriate national Standard shall be used. 2 5 EN ISO 4945:2009 (E) DIN EN ISO 4945:2010-03 to the condenser immediately after the addition of the sodium hydroxide Solution (5.5). Now begin the distillation. Distil about 80 ml in 25 min. Wh

41、en the distillation is ended, rinse the immersed tube with water (5.1), collecting the washings in the volumetric flask; make up to volume with water (5.1) and mix. Solutions S, for the 1 g test Portion and S, for the 2 g test Portion are obtained. Repeat the same Operation (8.3.2.1) for each Sample

42、 to be analysed, taking care, after each distillation, to rinse the flask with plenty of water, then distilled water and finally the water (5.1). NOTE - To regulate the boiling during the distillation in the apparatus shown in figure 1, it is as weil to add some pieces of porous ceramic. These piece

43、s are previously treated as a test Sample and collected up after distillation. They are then washed with sulphuric acid Solution (5.6) until neutral, then with water (5.1) and finally dried. 8.3.2.2 DISTILLATION UNDER A CURRENT OF STEAM Use the apparatus shown in figure 2 (6.2). To collect the disti

44、llate, transfer 5 ml of sulphuric acid (5.7) to a beaker of suitable capacity, introduce the tapered tube extension of the condenser into this beaker which has a mark at 85 ml, in such a manner that it is immersed in the 5 ml of sulphuric acid Solution (5.7). Pass the test Solution (8.3.1) quantitat

45、ively into the distillation flask with the aid of the funnel. Rinse the Kjeldahl flask with 60 ml of water (5.1), add through the funnel 50 ml of sodium hydroxide Solution (5.5) and rinse the funnel with 30 ml of water (5-l). The volume of the Solution should then be about 160 to 165 ml. The steam g

46、enerator should be preheated to allow the distillation to commence immediately the sodium hydroxide is introduced. Distil about 80 ml in 25 min. When the distillation is ended, rinse the immersed tube with water (5.1), collecting the washings in the beaker. Transfer the Solution quantitatively to a

47、100 ml one-mark volumetric flask, make up to volume with water (5.1) and mix. Solutions S, for the 1 g test Portion and S, for the 2 g test portion are obtained. Interrupt the heating of the steam generator and allow to cool; the liquid in the flask syphons into the empty flask. Repeat the same Oper

48、ation for each Sample to be analysed. 8.3.3 Development of the cofour According to the presumed nitrogen content, take the following aliquots of solutions S, and S, : - IO,0 ml for nitrogen contents between 0,020 and 0,050 % (mlm) - 25,0 ml for nitrogen contents between 0,010 and 0,020 % (mlm) - 50,

49、O ml for nitrogen contents between 0,002 and 0,010 % (mlm) and transfer them respectively into two 100 ml volumetric f lasks. Make up to 50 ml with water (5.1) those volumes less than 50 ml. Add 1 drop of methyl red Solution (5.15) and neutralize exactly with sodium hydroxide Solution (5.8). Add with a pipette and in the following Order : - 5,0 ml of sodium phenate Solution (5.9) - 5,0 ml of cCsodium hydrogen Phosphate solutil (5.10) - IO,0 ml of sodium pentacyanonitrosyIferrate( Solution (5.11) - 5,0 ml of sodium hypochlorite Solution (5.12). on Make up the volume