1、BRITISH STANDARD BSEN 10136:1991 Chemical analysis of ferrous materials Determination of nickel in steels and irons Flame atomic absorption spectrometric method This European Standard EN10136:1989 has the status of a BritishStandardBSEN10136:1991 This BritishStandard was published under the authorit
2、y ofthe Board of BSI and comes intoeffect on 31January1991 BSI12-1999 The following BSI references relate to the work on this standard: Committee reference ISM/18 Draft announced BSI News June1989 ISBN 0 580 19300 4 Cooperating organizations The European Committee for Standardization, under whose su
3、pervision this European Standard was prepared, comprises the national standards organizations of the following Western European countries. Austria Oesterreichisches Normungsinstitut Belgium Institut belge de normalisation Denmark Dansk Standardiseringsraad Finland Suomen Standardisoimisliito, r.y. F
4、rance Association franaise de normalisation Germany Deutsches Institut fr Normung e.V. Greece Hellenic Organization for Standardization Iceland Technological Institute of Iceland Ireland National Standards Authority of Ireland Italy Ente Nazionale Italiano di Unificazione Luxemburg Inspection du Tra
5、vail et des Mines Netherlands Nederlands Normalisatie-instituut Norway Norges Standardiseringsforbund Portugal Instituto Portugus da Qualidade Spain Asociacin Espaola de Normalizacin y Certificacin Sweden Standardiseringskommissionen i Sverige Switzerland Association suisse de normalisation United K
6、ingdom BritishStandards Institution Amendments issued since publication Amd. No. Date of issue CommentsBSEN10136:1991 BSI 12-1999 i Contents Page Cooperating organizations Inside front cover National foreword ii Brief history 2 Text of EN10136 3 National appendix NA Inside back coverBSEN10136:1991 i
7、i BSI 12-1999 National foreword This BritishStandard has been prepared under the direction of the Iron and Steel Standards Policy Committee. It is the English language version of EN10136:1989 “Chemical analysis of ferrous materials. Determination of nickel in steels and irons. Flame atomic absorptio
8、n spectrometric method”, published by the European Committee for Standardization (CEN). It supersedes BS6200-3.20.4:1986, which is withdrawn. Other methods for the determination of nickel in ferrous materials have been published as BS6200-3.20.1 andBS6200-3.20.3. NOTEThe text of the EN contains the
9、following minor typographical errors. These have been drawn to the attention of the appropriate Secretariat and will be corrected in the next edition of the EN. In5.1.1, lines2 and7, “absorbency” should read “absorbance”. In7.3.3, “Lamp current Slit width” should be directly opposite “Follow manufac
10、turers recommendations”. In7.3.5, lines6 and9, “absorbency” should read “absorbance”. In7.4, line5, “velues” should read “values”. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Comp
11、liance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pagesi andii, theEN title page, pages2 to8, an inside back cover and a back cover. This standard has been updated (see copyright da
12、te) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN10136 January1989 UDC 669.14:543.422:546.74 Key words: Iron- and steel products, steels, cast iron, chemical analysis, determinati
13、on of content, nickel, atomic absorption spectrophotometry, flame photometry. English version Chemical analysis of ferrous materials Determinationofnickel in steels and irons Flameatomicabsorption spectrometric method Analyse chimique des matriaux sidrurgiques Dosage du nickel dans les aciers et les
14、 fontes Mthode par spectromtrie dabsorption atomique dans la flamme Chemische Analyse von Eisenwerkstoffen Bestimmung von Nickel in Stahl Flammenatomabsorptionsspektrometrisches Verfahren This European Standard was accepted by CEN on15 January1989. CEN members are bound to comply with the requiremen
15、ts of the CEN/CENELEC Rules 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 Central Secretariat or t
16、o 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 Central Secretariat has the same status as the official ver
17、sions. CEN members are the national standards organizations of Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxemburg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and UnitedKingdom. CEN European Committee for Standardization Comit Europen de Nor
18、malisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels CEN 1989Copyright reserved to all CEN members Ref. No. EN 10136:1989EEN10136:1989 BSI 12-1999 2 Brief history This European Standard takes over the content of EURONORM136-85 “Chemical analysis of ferro
19、us materials Determination of nickel in steels and irons Flame atomic absorption spectrometric method”, prepared by ECISS/TC20 “Methods of chemical analysis”; the Secretariat of which is allocated to the Dansk Standardiseringsrad (DS). It has been submitted to the CEN Formal Vote following the decis
20、ion of the Coordinating Commission (COCOR) of the European Committeefor Iron and Steel Standardization on1987-11-24/25. It has been adopted and ratified by CEN BT on1988-11-05. According to the Common CEN/CENELEC Rules, following countries are bound to implement this European Standard: Austria, Belg
21、ium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxemburg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and UnitedKingdom. Note in clauses1 and9 EURONORM shall read EUROPEAN STANDARD. Contents Page Brief history 2 1 Scope and field of application 3 2 Reference 3
22、 3 Principle 3 4 Reagents 3 5 Apparatus 3 6 Sampling 4 7 Procedure 4 7.1 Test portion 4 7.2 Blank test 4 7.3 Determination 4 7.4 Establishment of the calibration graph 5 8 Expression of results 5 9 Test report 6 Annex Precision data 7EN10136:1989 BSI 12-1999 3 1 Scope and field of application This E
23、URONORM specifies a method for the determination of nickel in steels and irons by means of flame atomic absorption spectrometry. The method is applicable to steels and irons with nickel contents of0.003 to2.0% (m/m). 2 Reference EURONORM18 Selection and preparation of samples and test pieces for ste
24、el and iron and steel products. General guidelines for the application of flame atomic absorption spectrometric methods are in course of preparation. 3 Principle Dissolution of a test portion in a mixture of appropriate acids and fuming with perchloric acid. Spraying of the solution into an air-acet
25、ylene flame. Determination of the nickel by means of the spectrometric measurement of the atomic absorption of the232.0nm or352.5nm line emitted by a nickel hollow cathode lamp. The instrument is calibrated by addition of a nickel standard solution to a similar matrix to that of the test solution. N
26、OTEAt the wavelength of352.5nm the signal-to-noise ratio is higher than at a wavelength of232.0nm. Generally, use of the352.5nm line will lead to a better reproducibility. However, as the sensitivity at352.5nm is less than the sensitivity at232.0nm, with some instruments the use of the longer wavele
27、ngth will be impossible when analysing low nickel contents. 4 Reagents During the analysis use only reagents of recognized analytical reagent quality and having a very low nickel content, and only distilled water or water of equivalent purity. Carefully check the nickel content of all reagents. If p
28、ossible, use only freshly prepared distilled or deionized water. 4.1 Iron of high purity, with a nickel content0.0005% (m/m) 4.2 Hydrochloric acidnitric acid mixture Mix three volumes of hydrochloric acid, 1.19g/ml approximately, one volume of nitric acid, 1.40g/ml approximately and two volumes of w
29、ater. This mixture is to be prepared immediately before use. 4.3 Nitric acidperchloric acid mixture Mix100ml of nitric acid, 1.40g/ml approximately with800ml of perchloric acid, 1.54g/ml approximately. Dilute to1l with water and mix. NOTEPerchloric acid ( 1.67g/ml approximately) may also be used.100
30、ml of perchloric acid ( 1.54g/ml approximately) is equivalent to79ml of perchloric acid ( 1.67g/ml approximately). 4.4 Nickel stock solution, corresponding to1mg of nickel per ml approximately Weigh, to the nearest0.001g, about0.5g of high purity nickel (W 99.9% pure). Transfer the weighedmass to a4
31、00ml beaker and dissolve in25ml of nitric acid 1.40g/ml approximately diluted1+1 (v/v). Boil to remove oxides of nitrogen. Cool and transfer the solution to a500ml volumetric flask, dilute to the mark with water and mix. Calculate the concentration of nickel in this stock solution, in mg/ml. 4.5 Nic
32、kel reference solution, corresponding to40g of nickel per ml approximately Transfer10.0ml of nickel stock solution(4.4) to a250ml volumetric flask, dilute to the mark with water and mix. Calculate the concentration of nickel in the reference solution, in g/ml. 5 Apparatus Ordinary laboratory equipme
33、nt and 5.1 Atomic absorption spectrometer; a nickel hollow cathode lamp; supplies of air and acetylene sufficiently pure to give a steady clear fuel-lean flame, free from water and oil, and free from nickel The atomic absorption spectrometer used will be satisfactory if after optimization according
34、to7.3.4 the limit of detection and characteristic concentration are in reasonable agreement with the values given by the manufacturer and it meets the following performance requirements. 5.1.1 Minimum precision The standard deviation of10 measurements of the absorbency of the most concentrated solut
35、ion shall not exceed1.0% of the mean absorbance. The standard deviation of10 measurements of the absorbance of the least concentrated calibration solution (excluding the zero calibration solution) shall not exceed0.5% of the mean absorbency of the most concentrated calibration solution. For example,
36、 if the top and bottom calibration solutions represent0.1% and0.01% nickel in the sample, the precision called for (as two standard deviations) would be0.002% and0.001% nickel respectively, assuming curve linearity.EN10136:1989 4 BSI 12-1999 5.1.2 Additional performance requirements It is also desir
37、able that the instrument should conform to the following additional performance requirements. a) Characteristic concentration The characteristic concentration for nickel in a matrix similar to the final test solution shall be better than0.10g/ml. b) Limit of detection The limit of detection of nicke
38、l in a matrix similar to the final test solution shall be better than0.15g/ml. 5.2 Ancillary equipment A strip chart recorder and/or digital readout device is recommended to evaluate the criteria in5.1 and for all subsequent measurements. 6 Sampling Sampling shall be carried out in accordance with E
39、URONORM18. 7 Procedure WARNING Perchloric acid vapours may cause explosions in the presence of ammonia, nitrous fumes or organic matter in general. Always use a specially designed fume-hood. 7.1 Test portion Weigh the mass(m) indicated below to the nearest0.001g: m =1 g5%. 7.2 Blank test With each a
40、nalytical run, carry out an analysis on a reagent blank in parallel with the test portion analysis, using identical reagents, conditions, analytical procedures and dilutions throughout. 7.3 Determination 7.3.1 Preparation of the test solution Place the test portion(7.1) in a250ml beaker. Add10ml of
41、hydrochloric acidnitric acid mixture(4.2). Heat gently until the reaction ceases. Add15ml of nitric acidperchloric acid mixture(4.3) and heat until dense white fumes of perchloric acid appear. Continue heating for one minute and allow to cool. NOTEIf the test portion is readily soluble in the nitric
42、 acidperchloric acid mixture(4.3), the addition of hydrochloric acidnitric acid mixture(4.2) can be omitted. In that case the test portion is dissolved in the nitric acidperchloric acid mixture(4.3) and the solution thus obtained is heated as described above. Dissolve in25ml of water by heating gent
43、ly. Cool again and transfer the solution to a100ml volumetric flask, dilute to the mark with water and mix. This is the test solution. If some residue has been left in the solution due to silicon, tungsten, niobium or tantalum, filter the solution through a dry, medium textured filter paper, discard
44、ing the first runnings. If the expected nickel content of the test sample exceeds0.1% (m/m), dilute the solution as follows: Transfer25.0ml of the solution to a500ml volumetric flask, dilute to the mark with water and mix. NOTEIf the solution has to be diluted to give the test solution, the blank te
45、st solution(7.2) must be diluted in the same way. 7.3.2 Preparation of the calibration solutions Place10g of iron(4.1) in a800ml beaker. Add100ml of hydrochloric acidnitric acid mixture(4.2) and heat gently to dissolve the iron. Add150ml of nitric acidperchloric acid mixture(4.3) and heat until dens
46、e white fumes of perchloric acid appear. Continue heating for one minute and allow to cool. Dissolve in100ml of water by heating gently. Cool again and transfer the solution to a250ml volumetric flask, dilute to the mark with water and mix. 7.3.2.1 Nickel content 0.1% (m/m) Transfer a series of25.0m
47、l aliquots of the iron solution to100ml volumetric flasks, add to each flask by means of a burette or pipette respectively0,2.5,5.0,10.0,15.0,20.0 and25.0ml of nickel reference solution(4.5), dilute to the mark with water and mix. 7.3.2.2 Nickel content0.1 to2.0% (m/m) Transfer25.0ml of the iron sol
48、ution to a500ml volumetric flask, dilute to the mark with water and mix. From this solution transfer25.0ml aliquots to100ml volumetric flasks. Add to each flask by means of a burette or pipette respectively0,2.5,5.0,10.0,15.0,20.0 and25.0ml of nickel reference solution(4.5), dilute to the mark with
49、water and mix. NOTE1ml of nickel reference solution(4.5) is approximately equivalent to0.004% (m/m) in the sample in the case of7.3.2.1 and0.08% (m/m) in the sample in the case of7.3.2.2.EN10136:1989 BSI 12-1999 5 7.3.3 Adjustment of atomic absorption spectrometer(5.1) NOTEThe manufacturers recommendations should be closely followed and particular attention is drawn to the following safety points: a) the explosive nature of acetylene and regulations concerning its use; b) the need to shield the eyes of the ope
