Steel - Determination of nitrogen content - Spectrophotometric method (ISO 4945:1977)

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 can be converted to an ammonium salt.

Stahl - Bestimmung des Stickstoffgehalts - Spektralphotometrisches Verfahren (ISO 4945:1977)

Diese Internationale Norm legt ein spektralphotometrisches Verfahren zur Bestimmung des Stickstoffgehalts in unlegierten und niedrig legierten Stählen fest. Nach diesem Verfahren ist nur der Anteil des Stickstoffs zu bestimmen, der in ein Ammoniumsalz umgewandelt werden kann.

Acier - Dosage de l'azote - Méthode spectrophotométrique (ISO 4945:1977)

Jeklo - Določevanje dušika - Spektrometrična metoda (ISO 4945:1977)

Ta mednarodni standard opredeljuje spektrometrično metodo za določevanje dušika nelegiranega ali nizkolegiranega jekla. Ta metoda omogoča zgolj določevanje dušika, ki se lahko spremeni v amonijevo sol.

General Information

Status
Withdrawn
Publication Date
15-Dec-2009
Withdrawal Date
13-Dec-2018
Technical Committee
Current Stage
9900 - Withdrawal (Adopted Project)
Start Date
14-Dec-2018
Due Date
06-Jan-2019
Completion Date
14-Dec-2018

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Stahl - Bestimmung des Stickstoffgehalts - Spektralphotometrisches Verfahren (ISO 4945:1977)Acier - Dosage de l'azote - Méthode spectrophotométrique (ISO 4945:1977)Steel - Determination of nitrogen content - Spectrophotometric method (ISO 4945:1977)77.080.20JeklaSteels77.040.30Kemijska analiza kovinChemical analysis of metalsICS:Ta slovenski standard je istoveten z:EN ISO 4945:2009SIST EN ISO 4945:2010en01-januar-2010SIST EN ISO 4945:2010SLOVENSKI
STANDARD



SIST EN ISO 4945:2010



EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN ISO 4945
October 2009 ICS 77.080.20 English Version
Steel - Determination of nitrogen content - Spectrophotometric method (ISO 4945:1977)
Acier - Dosage de l'azote - Méthode spectrophotométrique (ISO 4945:1977)
Stahl - Bestimmung des Stickstoffgehalts - Spektralphotometrisches Verfahren (ISO 4945:1977) This European Standard was approved by CEN on 5 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 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 into 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, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2009 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 4945:2009: ESIST EN ISO 4945:2010



EN ISO 4945:2009 (E) 2 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 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 April 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 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, 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.
SIST EN ISO 4945:2010



w - INTERNATIONAL STANDARD - INTERNATIONAL ORGANIZATION FOR STANDARDIZATION l MEXAYHAPOAHAII OPI-AHWSALWI l-IO CTAH~APTM3ALJWW .ORGANISATION INTERNATIONALE DE NORMALISATION Steel - Determination of nitrogen content - Spectrophotometric method Acier - Dosage de Kazote - Methode spectropho tombrique First edition - 1977-12-15 Corrected and reprinted - UDC 669.14 : 669.786 : 543.42 Ref. No. ISO 4945-1977 (E) Descriptors : steels, Chemical analysis, determination of content, nitrogen, spectrophotometric analysis. Price based on 6 pages SIST EN ISO 4945:2010



FOREWORD . ISO (the International Organization for Standardization) is a worldwide federation of national Standards institutes (ISO member bodies). The work of developing International Standards is carried out through ISO technical committees. Every member body interested in a subject for which a technical committee has been set up 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. Draft International Standards adopted by the technical committees are circulated to the member bodies for approval before their acceptance as International Standards by the ISO Council. International Standard ISO 4945 was developed by Technical Committee ISO/TC 17, Steel, and was circulated to the member bodies in March 1976. lt has been approved by the member bodies of the following countries : Australia Belgium Canada Chile Czechoslovakia Denmark Finland France Germany Hungary India Iran Ireland Italy Korea, Rep. of Mexico Netherlands Norway Philippines Poland The member bodies of the following document on technical grounds : countries expressed disapproval of the Australia Japan 0 International Organization for Standardization, 1977 l Printed in Switzerland Portugal South Africa, Rep. of Spain Sweden Switzerland Turkey U.S.A. U.S.S. R. Yugoslavia SIST EN ISO 4945:2010



INTERNATIONAL STANDARD ISO 4945-1977 (E) Steel - Determination of nitrogen content - Spectrophotometric method 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 FIELD 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 test 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, formation 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 only 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 nitrogen 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. Dissolve, 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 acid, 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 mix. 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 Solution 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 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) SIST EN ISO 4945:2010



ISO 4945-1977 (E) dihydrate (sodium nitroprusside) [Na, Fe (CN), N0.2H,O] in water (5.1), make up the 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 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 inci- derice of the value of the blank test when the same reagents are used with th
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