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1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS EN 10211 : 1996 The Eu
2、ropean Standard EN 10211 : 1995 has the status of a British Standard ICS 77.080 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Chemical analysis of ferrous materials Determination of titanium in steel and iron Flame atomic absorption spectrometric method Licensed Copy: sheffi
3、eldun sheffieldun, na, Thu Oct 26 04:14:06 GMT+00:00 2006, Uncontrolled Copy, (c) BSI This British Standard, having been prepared under the direction of the Engineering Sector Board, was published under the authority of the Standards Board and comes into effect on 15 August 1996 BSI 1996 The followi
4、ng BSI references relate to the work on this standard: Committee reference ISE/18 Draft for comment 91/37094 DC ISBN 0 580 25769 X BS EN 10211 : 1996 Amendments issued since publication Amd. No.DateText affected Committees responsible for this British Standard The preparation of this British Standar
5、d was entrusted to Technical Committee ISE/18, Sampling and analysis of iron and steel, upon which the following bodies were represented: BCIRA British Iron and Steel Producers Association Ministry of Defence Welding Institute Coopted members Licensed Copy: sheffieldun sheffieldun, na, Thu Oct 26 04
6、:14:06 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN 10211 : 1996 BSI 1996i Contents Page Committees responsibleInside front cover National forewordii Foreword2 Text of EN 102113 Licensed Copy: sheffieldun sheffieldun, na, Thu Oct 26 04:14:06 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ii BSI 1996
7、 BS EN 10211 : 1996 National foreword This British Standard has been prepared by Technical Committee ISE/18 and is the English language version of EN 10211 : 1995 Chemical analysis of ferrous materials Determination of titanium in steel and iron Flame atomic absorption spectrometric method published
8、 by the European Committee for Standardization (CEN). Cross-references Publication referred toCorresponding British Standard BS 6200 Sampling and analysis of iron, steel and other ferrous metals Part 6 Guidelines on atomic absorption spectrometric techniques Information Circular No. 8 BS 6200 : Sect
9、ion 6.1 : 1990 Recommendations for the drafting of standard methods for the chemical analysis of iron and steel by flame atomic absorption spectrometry Compliance with a British Standard does not of itself confer immunity from legal obligations. Licensed Copy: sheffieldun sheffieldun, na, Thu Oct 26
10、 04:14:06 GMT+00:00 2006, Uncontrolled Copy, (c) BSI CEN European Committee for Standardization Comite Europe en de Normalisation Europa isches Komitee fu r Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1995 All rights of reproduction and communication in any form and by any means
11、 reserved in all countries to CEN and its members Ref. No. EN 10211 : 1995 E EUROPEAN STANDARDEN 10211 NORME EUROPE ENNE EUROPA ISCHE NORM October 1995 ICS 77.080.00 Descriptors: Iron- and steel products, steels, cast iron, chemical analysis, determination of content, titanium, atomic absorption spe
12、ctrophotometry, flame photometry English version Chemical analysis of ferrous materials Determination of titanium in steel and iron Flame atomic absorption spectrometric method Analyse chimique des mate riaux side rurgiques Dosage du titane dans les aciers et les fontes Me thode par spectrome trie d
13、absorption atomique Chemische Analyse der Eisen- und Stahlwerkstoffe Bestimmung des Titaniumgehaltes in Stahl und Eisen Flammenatomabsorptionspektrometrisches Verfahren This European Standard was approved by CEN on 1995-07-14. CEN members are bound to comply with the CEN/CENELEC Internal Regulations
14、 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 Central Secretariat or to any CEN member. This European
15、 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 Central Secretariat has the same status as the official versions. CEN members are the national
16、 standards bodies of Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. Licensed Copy: sheffieldun sheffieldun, na, Thu Oct 26 04:14:06 GMT+00:00 2006, Uncontrolled Copy, (c)
17、BSI Page 2 EN 10211: 1995 BSI 1996 Foreword This European Standard was prepared by Technical Committee, ECISS/TC 20, Methods of chemical analysis, of which the secretariat is held by SIS. This European Standard shall be given the status of a national standard, either by publication of an identical t
18、ext or by endorsement, at the latest by April 1996, and conflicting national standards shall be withdrawn at the latest by April 1996. In accordance with CEN/CENELEC Internal Regulations, the following countries are bound to implement this European Standard: Austria, Belgium, Denmark, Finland, Franc
19、e, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland, United Kingdom. Contents Page Foreword2 1Scope3 2Normative references3 3Principle3 4Reagents3 5Apparatus4 6Sampling4 7Procedure4 8Expression of results6 9Test report6 Annex A (informat
20、ive) Precision data7 Licensed Copy: sheffieldun sheffieldun, na, Thu Oct 26 04:14:06 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 3 EN 10211: 1995 BSI 1996 1 Scope This European Standard specifies a flame atomic absorption spectrometric method for the determination of titanium in steel and iron.
21、The method is applicable to alloyed and non-alloyed steel and iron with titanium contents of 0,01 % to 1 % (m/m). 2 Normative references This European Standard incorporates by dated or undated reference, provisions from other publications. These normative references are cited at the appropriate plac
22、es in the text and the publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incorporated in it by amendment or revision. For undated references the latest edition of the publication refer
23、red to applies. EURONORM 18:Selection and preparation of samples and test pieces for steel and iron and steel products INFORMATION CIRCULAR No. 8: Recommendations for the drafting of standard methods of analysis employing flame atomic absorption spectrometry for the chemical analysis of iron and ste
24、el INFORMATION CIRCULAR No. 9: Operational guidelines for the application of flame atomic absorption spectrometry in standard methods for the chemical analysis of iron and steel 3 Principle Two dissolution procedures are possible: 3.1 Dissolution with nitric and perchloric acid Separation of the sil
25、ica by filtration, after rendering insoluble by evaporation to dryness in perchloric medium. 3.2 Dissolution with hydrochloric and nitric acid and recovery of the residue by fusion with a mixture of sodium carbonate and boric acid Addition of aluminium chloride as interaction buffer. Nebulization of
26、 the solution in a nitrous oxide-acetylene flame, slightly fuel rich, and comparison of the absorbance of the resonance energy of the titanium present in the test solution with that in the calibration solutions. Recommended wavelength: 365,3 nm (or 364,3 nm) 4 Reagents During the analysis, use only
27、reagents of recognized analytical reagent quality and having a very low titanium content, and only distilled water or water of equivalent purity. 4.1 Nitric acid, approximately 1,40 g/ml. 4.2 Hydrochloric acid, approximately 1,19 g/ml. 4.3 Perchloric acid, approximately 1,67 g/ml. 4.4 Sulfuric acid,
28、 approximately 1,84 g/ml. 4.5 Hydrofluoric acid, approximately 1,15 g/ml. 4.6 Nitric acid, approximately 1,40 g/ml, diluted 1 + 1. 4.7 Hydrochloric acid, approximately 1,19 g/ml, diluted 1 + 1. 4.8 Aluminium chloride solution, equivalent to 10 g/l Al. Dissolve 90 g of hydrated aluminium chloride (Al
29、Cl3.6H2O) in water. Transfer to a 1000 ml flask. Make up to volume with water and mix. 4.9 Flux mixture. Mix intimately one part of sodium carbonate (Na2CO3) with an equal part by mass of boric acid (H3BO3). Store in a stoppered polyethylene container. 4.10 Iron, 20 g/l perchloric solution. Weigh to
30、 the nearest 0,01 g, 10 g of pure iron free of titanium or of known low titanium content. Place in a 600 ml beaker and cover with a watch glass. Add, in small amounts, 150 ml of nitric acid (4.6). After effervescence ceases, add 200 ml of perchloric acid (4.3). Heat gently to complete the attack. Wh
31、en this is finished, raise the temperature to white perchloric fumes and continue heating until crystallization of iron perchlorate. Allow to cool. Take up in about 150 ml of water. Swirl to dissolve the salts, bring gently to the boil. Cool. Transfer quantitatively to a 500 ml volumetric flask. Mak
32、e up to volume with water and mix. 4.11 Iron, 20 g/l chloro-nitric solution. Weigh to the nearest 0,01 g, 20 g of pure iron free of titanium or of known titanium content. Place in a 600 ml tall form beaker, then add 200 ml of water and gradually 220 ml of hydrochloric acid (4.2). Cover with a watch
33、glass and heat carefully until dissolution is complete. After effervescence ceases, add gradually 60 ml of nitric acid (4.1). Heat for 10 min at about 80 C to eliminate nitrous fumes. Remove from the heat and allow to cool. Transfer to a 1000 ml volumetric flask. Dilute to about 600 ml. Add 20 g of
34、flux mixture (4.9). Dissolve, make up to volume with water and mix. 4.12 Titanium, 1 g/l standard solution. Weigh to the nearest 0,001 g, 1 g of pure titanium (99,99 %). Place in a 400 ml beaker, cover with a watch glass. Dissolve in 200 ml hydrochloric acid (4.7); add two drops of hydrofluoric acid
35、 (4.5). Heat to complete the dissolution. Cool. Transfer the solution quantitatively to a 1000 ml volumetric flask. Make up to volume with water and mix. 1 ml of this standard solution contains 1 mg of titanium. Licensed Copy: sheffieldun sheffieldun, na, Thu Oct 26 04:14:06 GMT+00:00 2006, Uncontro
36、lled Copy, (c) BSI Page 4 EN 10211: 1995 BSI 1996 4.13 Titanium, 0,05 g/l standard solution (to be prepared immediately before use). Take exactly 10 ml of the titanium standard solution (4.12). Place in a 200 ml volumetric flask. Make up to volume with water and mix. 1 ml of this standard solution c
37、ontains 0,05 mg of titanium. 4.14 Titanium, 0,5 g/l standard solution (to be prepared immediately before use). Take exactly 50 ml of the titanium standard solution (4.12). Place in a 100 ml volumetric flask. Make up to volume with water and mix. 1 ml of this standard solution contains 0,5 mg of tita
38、nium. 5 Apparatus Ordinary laboratory equipment and 5.1 30 ml platinum crucible 5.2 Atomic absorption spectrometer, a titanium hollow cathode lamp; supplies of nitrous oxide and acetylene sufficiently pure to give a clear, steady slightly fuel-rich flame, free of water, oil and of titanium. The atom
39、ic absorption spectrometer used will be satisfactory if, after optimization according to 7.6, 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. 5.2.1 Minimum precision The
40、 standard deviation of 10 measurements of the absorbance of the most concentrated calibration solution shall not exceed 1,5 % of the mean absorbance. The standard deviation of 10 measurements of the absorbance of the least concentrated calibration solution (excluding the zero calibration solution) s
41、hall not exceed 0,5 % of the mean absorbance of the most concentrated calibration solution. 5.2.2 Additional performance requirements It is also desirable that the instrument should conform to the following additional performance requirements (see clause 2 of Information Circular No. 8). a) Characte
42、ristic concentration. The characteristic concentration for titanium in a matrix similar to the final test portion solution shall be better than 1,9 mg/ml for the 365,3 nm line and better than 1,4 mg/ml for the 364,3 nm line. b) Limit of detection. The limit of detection of titanium in a matrix simil
43、ar to that of the final test portion solution shall be better than 0,2 mg/ml for the 365,3 nm line and better than 0,1 mg/ml for the 364,3 nm line. 5.2.3 Ancillary equipment A strip chart recorder and/or digital readout device is recommended to evaluate the criteria in 5.2 and for all subsequent mea
44、surements. 6 Sampling Sampling shall be carried out in accordance with EURONORM 18. 7 Procedure 7.1 Test portion Weigh, to the nearest 0,001 g, a test portion of 1 g0,01 g. 7.2 Blank test With each analytical run, carry out a blank analysis in parallel with the test portion analysis, using identical
45、 reagents, conditions, analytical procedures in accordance with the chosen dissolution method, 7.3.1 or 7.3.2, and dilutions throughout, including iron (solution 4.10 or 4.11 depending on the chosen dissolution). 7.3 Preparation of the test solution 7.3.1 Nitric perchloric dissolution Place the test
46、 portion (7.1) in a 250 ml beaker. Cover with watch glass. Add 15 ml of nitric acid (4.6). After effervescence ceases, add 20 ml of perchloric acid (4.3). Heat gently to complete the attack. Then raise the temperature to white perchloric fumes and continue heating until crystallization of iron perch
47、lorate. Allow to cool. Take up in 25 ml to 30 ml of water. Boil gently for a few minutes. Filter the silica, wash with hot water collecting the filtrate and the washings in a 100 ml volumetric flask. Cool. Add 5 ml of aluminium chloride solution (4.8). Make up to volume with water and mix. 7.3.2 Chl
48、oro-nitric dissolution with recovery of the residue Place the test portion in a 150 ml narrow necked conical flask. Add 20 ml of hydrochloric acid (4.7), cover with a watch glass and heat carefully until dissolution is complete. After effervescence ceases, add gently 3 ml of nitric acid (4.1). Heat
49、for 10 min at about 80 C to expel nitrous fumes. Remove from the heat and allow to cool. Filter through a dry filter collecting the filtrate in a 100 ml volumetric flask. Wash the residue on the filter with boiling water (about 40 ml). Place the filter containing the residue in a platinum crucible (5.1). Cover with a platinum lid. Place the covered crucible progressively into a muffle furnace set at 900 C in order to ash the filter and the residue. Leave 15 min, then remove and allow to cool. Add 2 drops of sulfuric acid (4.4) and about 2 ml of h
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