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1、BRITISH STANDARD BS EN 10136:1991 Chemical analysis of ferrous materials Determination of nickel in steels and irons Flame atomic absorption spectrometric method This European Standard EN 10136:1989 has the status of a British Standard BS EN 10136:1991 This British Standard was published under the a
2、uthority of the Board of BSI and comes into effect on 31 January 1991 BSI 12-1999 The following BSI references relate to the work on this standard: Committee reference ISM/18 Draft announced BSI News June 1989 ISBN 0 580 19300 4 Cooperating organizations The European Committee for Standardization, u
3、nder whose supervision this European Standard was prepared, comprises the national standards organizations of the following Western European countries. AustriaOesterreichisches Normungsinstitut BelgiumInstitut belge de normalisation DenmarkDansk Standardiseringsraad FinlandSuomen Standardisoimisliit
4、o, r.y. FranceAssociation franaise de normalisation GermanyDeutsches Institut fr Normung e.V. GreeceHellenic Organization for Standardization IcelandTechnological Institute of Iceland IrelandNational Standards Authority of Ireland ItalyEnte Nazionale Italiano di Unificazione LuxemburgInspection du T
5、ravail et des Mines NetherlandsNederlands Normalisatie-instituut NorwayNorges Standardiseringsforbund PortugalInstituto Portugus da Qualidade SpainAsociacin Espaola de Normalizacin y Certificacin SwedenStandardiseringskommissionen i Sverige SwitzerlandAssociation suisse de normalisation United Kingd
6、omBritish Standards Institution Amendments issued since publication Amd. No.Date of issueComments BS EN 10136:1991 BSI 12-1999i Contents Page Cooperating organizationsInside front cover National forewordii Brief history2 Text of EN 101363 National appendix NAInside back cover BS EN 10136:1991 ii BSI
7、 12-1999 National foreword This British Standard has been prepared under the direction of the Iron and Steel Standards Policy Committee. It is the English language version of EN 10136:1989 “Chemical analysis of ferrous materials. Determination of nickel in steels and irons. Flame atomic absorption s
8、pectrometric method”, published by the European Committee for Standardization (CEN). It supersedes BS 6200-3.20.4:1986, which is withdrawn. Other methods for the determination of nickel in ferrous materials have been published as BS 6200-3.20.1 and BS 6200-3.20.3. 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. In 5.1.1, lines 2 and 7, “absorbency” should read “absorbance”. In 7.3.3, “Lamp current Slit width” should be directly opposite “Follow ma
10、nufacturers recommendations”. In 7.3.5, lines 6 and 9, “absorbency” should read “absorbance”. In 7.4, line 5, “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 applica
11、tion. Compliance 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, pages i and ii, the EN title page, pages 2 to 8, an inside back cover and a back cover. This standard has been updated (s
12、ee copyright date) 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 EN 10136 January 1989 UDC 669.14:543.422:546.74 Key words: Iron- and steel products, steels, cast iron, chemical ana
13、lysis, determination of content, nickel, atomic absorption spectrophotometry, flame photometry. English version Chemical analysis of ferrous materials Determination of nickel in steels and irons Flame atomic absorption spectrometric method Analyse chimique des matriaux sidrurgiques Dosage du nickel
14、dans les aciers et les 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 on 15 January 1989. CEN members are bound to co
15、mply with the requirements 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
16、Central Secretariat 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 Central Secretariat has the same st
17、atus as the official versions. 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 United Kingdom. CEN European Committee for Standardiza
18、tion Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels CEN 1989 Copyright reserved to all CEN members Ref. No. EN 10136:1989 E EN 10136:1989 BSI 12-1999 2 Brief history This European Standard takes over the content of EURONORM 136-
19、85 “Chemical analysis of ferrous materials Determination of nickel in steels and irons Flame atomic absorption spectrometric method”, prepared by ECISS/TC 20 “Methods of chemical analysis”; the Secretariat of which is allocated to the Dansk Standardiseringsrad (DS). It has been submitted to the CEN
20、Formal Vote following the decision of the Coordinating Commission (COCOR) of the European Committee for Iron and Steel Standardization on 1987-11-24/25. It has been adopted and ratified by CEN BT on 1988-11-05. According to the Common CEN/CENELEC Rules, following countries are bound to implement thi
21、s European Standard: Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxemburg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. Note in clauses 1 and 9 EURONORM shall read EUROPEAN STANDARD. Contents Page Brief history2 1Scope and f
22、ield of application3 2Reference3 3Principle3 4Reagents3 5Apparatus3 6Sampling4 7Procedure4 7.1Test portion4 7.2Blank test4 7.3Determination4 7.4Establishment of the calibration graph5 8Expression of results5 9Test report6 Annex Precision data7 EN 10136:1989 BSI 12-19993 1 Scope and field of applicat
23、ion This EURONORM 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 of 0.003 to 2.0 % (m/m). 2 Reference EURONORM 18 Selection and preparation of samples and test
24、pieces for steel 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 in
25、to an air-acetylene flame. Determination of the nickel by means of the spectrometric measurement of the atomic absorption of the 232.0 nm or 352.5 nm 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 th
26、e test solution. NOTEAt the wavelength of 352.5 nm the signal-to-noise ratio is higher than at a wavelength of 232.0 nm. Generally, use of the 352.5 nm line will lead to a better reproducibility. However, as the sensitivity at 352.5 nm is less than the sensitivity at 232.0 nm, with some instruments
27、the use of the longer wavelength 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 c
28、ontent of all reagents. If possible, use only freshly prepared distilled or deionized water. 4.1 Iron of high purity, with a nickel content 0.0005 % (m/m) 4.2 Hydrochloric acidnitric acid mixture Mix three volumes of hydrochloric acid, 1.19 g/ml approximately, one volume of nitric acid, 1.40 g/ml ap
29、proximately and two volumes of water. This mixture is to be prepared immediately before use. 4.3 Nitric acidperchloric acid mixture Mix 100 ml of nitric acid, 1.40 g/ml approximately with 800 ml of perchloric acid, 1.54 g/ml approximately. Dilute to 1 l with water and mix. NOTEPerchloric acid ( 1.67
30、 g/ml approximately) may also be used. 100 ml of perchloric acid ( 1.54 g/ml approximately) is equivalent to 79 ml of perchloric acid ( 1.67 g/ml approximately). 4.4 Nickel stock solution, corresponding to 1 mg of nickel per ml approximately Weigh, to the nearest 0.001 g, about 0.5 g of high purity
31、nickel (W 99.9 % pure). Transfer the weighed mass to a 400 ml beaker and dissolve in 25 ml of nitric acid 1.40 g/ml approximately diluted 1 + 1 (v/v). Boil to remove oxides of nitrogen. Cool and transfer the solution to a 500 ml volumetric flask, dilute to the mark with water and mix. Calculate the
32、concentration of nickel in this stock solution, in mg/ml. 4.5 Nickel reference solution, corresponding to 40 g of nickel per ml approximately Transfer 10.0 ml of nickel stock solution (4.4) to a 250 ml volumetric flask, dilute to the mark with water and mix. Calculate the concentration of nickel in
33、the reference solution, in g/ml. 5 Apparatus Ordinary laboratory equipment 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
34、 spectrometer used will be satisfactory if after optimization according to 7.3.4 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 dev
35、iation of 10 measurements of the absorbency of the most concentrated solution shall not exceed 1.0 % of the mean absorbance. The standard deviation of 10 measurements of the absorbance of the least concentrated calibration solution (excluding the zero calibration solution) shall not exceed 0.5 % of
36、the mean absorbency of the most concentrated calibration solution. For example, if the top and bottom calibration solutions represent 0.1 % and 0.01 % nickel in the sample, the precision called for (as two standard deviations) would be 0.002 % and 0.001 % nickel respectively, assuming curve linearit
37、y. EN 10136:1989 4 BSI 12-1999 5.1.2 Additional performance requirements It is also desirable 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 sol
38、ution shall be better than 0.10 g/ml. b) Limit of detection The limit of detection of nickel in a matrix similar to the final test solution shall be better than 0.15 g/ml. 5.2 Ancillary equipment A strip chart recorder and/or digital readout device is recommended to evaluate the criteria in 5.1 and
39、for all subsequent measurements. 6 Sampling Sampling shall be carried out in accordance with EURONORM 18. 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 porti
40、on Weigh the mass (m) indicated below to the nearest 0.001 g: m = 1 g 5 %. 7.2 Blank test With each analytical 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 Determina
41、tion 7.3.1 Preparation of the test solution Place the test portion (7.1) in a 250 ml beaker. Add 10 ml of hydrochloric acidnitric acid mixture (4.2). Heat gently until the reaction ceases. Add 15 ml of nitric acidperchloric acid mixture (4.3) and heat until dense white fumes of perchloric acid appea
42、r. Continue heating for one minute and allow to cool. NOTEIf the test portion is readily soluble in the nitric 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 mi
43、xture (4.3) and the solution thus obtained is heated as described above. Dissolve in 25 ml of water by heating gently. Cool again and transfer the solution to a 100 ml volumetric flask, dilute to the mark with water and mix. This is the test solution. If some residue has been left in the solution du
44、e to silicon, tungsten, niobium or tantalum, filter the solution through a dry, medium textured filter paper, discarding the first runnings. If the expected nickel content of the test sample exceeds 0.1 % (m/m), dilute the solution as follows: Transfer 25.0 ml of the solution to a 500 ml volumetric
45、flask, dilute to the mark with water and mix. NOTEIf the solution has to be diluted to give the test solution, the blank test solution (7.2) must be diluted in the same way. 7.3.2 Preparation of the calibration solutions Place 10 g of iron (4.1) in a 800 ml beaker. Add 100 ml of hydrochloric acidnit
46、ric acid mixture (4.2) and heat gently to dissolve the iron. Add 150 ml 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. Dissolve in 100 ml of water by heating gently. Cool again and transfer th
47、e solution to a 250 ml volumetric flask, dilute to the mark with water and mix. 7.3.2.1 Nickel content 0.1 % (m/m) Transfer a series of 25.0 ml aliquots of the iron solution to 100 ml volumetric flasks, add to each flask by means of a burette or pipette respectively 0, 2.5, 5.0, 10.0, 15.0, 20.0 and
48、 25.0 ml of nickel reference solution (4.5), dilute to the mark with water and mix. 7.3.2.2 Nickel content 0.1 to 2.0 % (m/m) Transfer 25.0 ml of the iron solution to a 500 ml volumetric flask, dilute to the mark with water and mix. From this solution transfer 25.0 ml aliquots to 100 ml volumetric f
49、lasks. Add to each flask by means of a burette or pipette respectively 0, 2.5, 5.0, 10.0, 15.0, 20.0 and 25.0 ml of nickel reference solution (4.5), dilute to the mark with water and mix. NOTE1 ml of nickel reference solution (4.5) is approximately equivalent to 0.004 % (m/m) in the sample in the case of 7.3.2.1 and 0.08 % (m/m) in the sample in the case of 7.3.2.2. EN 10136:1989 BSI 12-19995 7.3.3 Adjustment of atomic absorption spectrometer (5.1) NOTEThe manufacturers recommendations should be closely fol