1、BRITISH STANDARD BS EN ISO 10700:1995 Steel and iron Determination of manganese content Flame atomic absorption spectrometric method The European Standard EN ISO 10700:1995 has the status of a British StandardBSENISO10700:1995 This British Standard, having been prepared under the directionof the Eng
2、ineering SectorBoard, was published underthe authority of the Standards Board and comes into effect on 15December1995 BSI 01-2000 The following BSI references relate to the work on this standard: Committee reference ISE/18 Draft for comment 93/300209 DC ISBN 0 580 25014 8 Committees responsible for
3、this British Standard The preparation of this British Standard was entrusted to Technical Committee ISE/18, Sampling and analysis of iron and steel, upon which the following bodies were represented: British Cast Iron Research Association British Iron and Steel Producers Association Ministry of Defen
4、ce The Welding Institute Amendments issued since publication Amd. No. Date CommentsBSENISO10700:1995 BSI 01-2000 i Contents Page Committees responsible Inside front cover National foreword ii Foreword 2 1 Scope 3 2 Normative references 3 3 Principle 3 4 Reagents 3 5 Apparatus 3 6 Sampling 4 7 Proced
5、ure 4 8 Expression of results 7 9 Test report 7 Annex A (normative) Procedures for the determination of instrumental criteria 8 Annex B (informative) Additional information on the international co-operative tests 10 Annex C (informative) Graphical representation of precision data 11 Annex ZA (normat
6、ive) Normative references to international publications with their relevant European publications 12 Figure A.1 9 Figure C.1 Logarithmic relationship between manganese content (w Mn ) and repeatability (r) or reproducibility (R and R w ) 11 Table 1 5 Table 2 5 Table 3 5 Table 4 6 Table 5 7 Table B.1
7、 10 List of references Inside back coverBSENISO10700:1995 ii BSI 01-2000 National foreword This British Standard has been prepared by Technical Committee ISE/18 and is the English language version of ENISO10700:1995 Steel and iron Determination of manganese content Flame atomic absorption spectromet
8、ric method, published by the European Committee for Standardization (CEN). ENISO10700 is identical with ISO10700:1994, published by the International Organization for Standardization (ISO). It was produced as a result of international discussions in which the United Kingdom took an active part. A Br
9、itish Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Cross-references Publication referred to Corr
10、esponding British Standard ISO 1042:1983 BS 1792:1982 Specification for one-mark volumetric flasks ISO 3696:1987 BS 3978:1987 Specification for water for laboratory use ISO 5725:1986 BS 5497 Precision of test methods Part 1:1987 Guide for the determination of repeatability and reproducibility for a
11、standard test method by inter-laboratory tests Summary of pages This document comprises a front cover, an inside front cover, pagesi andii, the EN ISO title page, pages2to12, an inside back cover and a back cover. This standard has been updated (see copyright date) and may have had amendments incorp
12、orated. This will be indicated in the amendment table on the inside front cover.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 10700 September 1995 ICS 77.080 Descriptors: Steels, iron, chemical analysis, determination of content, manganese, atomic absorption spectrometric method English v
13、ersion Steel and ironDeterminationof manganese content Flame atomic absorption spectrometric method (ISO 10700:1994) Aciers et fontes Dosage du manganse Mthode par spectromtrie dabsorption atomique dans la flamme (ISO 10700:1994) Stahl und Eisen Bestimmung von Mangan Flammenatomabsorptionsspektromet
14、risches Verfahren (ISO 10700:1994) This European Standard was approved by CEN on1995-08-06. 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
15、lists and bibliographical references concerning such national standards may be obtained on application to the 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 re
16、sponsibility 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 standards bodies of Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Nor
17、way, Portugal, Spain, Sweden, Switzerland and United Kingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1995 All rights of reproduction and communication in any form and by any mea
18、ns reserved in all countries to CEN and its members Ref. No. EN ISO 10700:1995 EENISO10700:1995 BSI 01-2000 2 Foreword The text of the International Standard from ISO/TC17, Steel, of the International Organization for Standardization (ISO) has been taken over as a European Standard by the Technical
19、Committee ECISS/TC20, Methods of chemical analysis. 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 March1996, and conflicting national standards shall be withdrawn at the latest March1996. According
20、 to the CEN/CENELEC Internal Regulations, the following countries are bound to implement this European Standard: Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom.ENISO107
21、00:1995 BSI 01-2000 3 1 Scope This International Standard specifies a flame atomic absorption spectrometric method for the determination of the manganese content in steel and iron. The method is applicable to manganese contents between0,002% (m/m) and2,0% (m/m). 2 Normative references The following
22、standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this International Standard are encourage
23、d to investigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 377-2:1989, Selection and preparation of samples and test pieces of wrought steels Part2:Samples for the d
24、etermination of the chemical composition. ISO 385-1:1984, Laboratory glassware Burettes Part 1: General requirements. ISO 648:1977, Laboratory glassware One-mark pipettes. ISO 1042:1983, Laboratory glassware One-mark volumetric flasks. ISO 3696:1987, Water for analytical laboratory use Specification
25、 and test methods. ISO 5725:1986, Precision of test methods Determination of repeatability and reproducibility for a standard test method by inter-laboratory tests. 3 Principle Dissolution of a test portion in hydrochloric and nitric acids followed by evaporation with perchloric acid until white fum
26、es appear. Spraying of the solution into an air-acetylene flame. Spectrometric measurement of the atomic absorption of the279,5 nm spectral line emitted by a manganese hollow cathode lamp. 4 Reagents During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and o
27、nly grade2water as specified in ISO3696. 4.1 Pure iron, free from manganese or with a known low manganese content. 4.2 Hydrochloric acid, about1,19g/ml. 4.3 Hydrofluoric acid, about1,15g/ml. 4.4 Nitric acid, about1,40g/ml. 4.5 Perchloric acid, about1,54g/ml (see note1). NOTE 1Perchloric acid ( about
28、1,67g/ml) may also be used. 100ml of perchloric acid ( about1,54g/ml) is equivalent to79ml of perchloric acid ( about1,67g/ml). 4.6 Background solution WARNING See clause7. Weigh, to the nearest0,01g, 10,00g of the pure iron(4.1). Place in a1litre beaker. Add200ml of hydrochloric acid (4.2), cover t
29、he beaker with a watch glass and heat gently until the iron is dissolved. Then oxidize by adding50ml of nitric acid (4.4) in small portions. Add150ml of perchloric acid (4.5). Heat strongly and evaporate until dense white fumes of perchloric acid appear. Continue fuming for15min at a temperature tha
30、t maintains a steady reflux of white perchloric acid fumes on the walls of the beaker. Allow to cool, add300ml of water and heat gently to dissolve the salts. Transfer quantitatively to a1000ml one-mark volumetric flask. Dilute to the mark with water and mix. 1ml of this background solution contains
31、0,010g of Fe. 4.7 Manganese, standard solution 4.7.1 Manganese stock solution, corresponding to1,00g of Mn per litre. Weigh, to the nearest0,1mg, 1,00g of pure manganese metal purity W 99,9% (m/m). Place ina250ml beaker and add40ml of hydrochloric acid(4.2). Cover with a watch glass and heat gently
32、until the manganese has dissolved. Cool, transfer the solution quantitatively to a1000ml one-mark volumetric flask, dilute to the mark with water and mix. 1ml of this standard solution contains1,00mg of Mn. 4.7.2 Manganese standard solution, corresponding to 0,02g of Mn per litre. Transfer20,0ml of
33、the stock solution (4.7.1) toa1000ml one-mark volumetric flask, dilute to the mark with water and mix. Prepare this standard solution immediately before use. 1ml of this standard solution contains0,02mg of Mn. 5 Apparatus All volumetric glassware shall be class A, in accordance with ISO385-1, ISO648
34、 or ISO1042, as appropriate. Ordinary laboratory apparatus, andENISO10700:1995 4 BSI 01-2000 5.1 Atomic absorption spectrometer, equipped with a manganese hollow cathode lamp and supplied with air and acetylene sufficiently pure to give a steady clear fuel-lean flame, free from water and oil, and fr
35、ee from manganese. The atomic absorption spectrometer used will be satisfactory if, after optimization according to7.3.5, the limit of detection and characteristic concentration are in reasonable agreement with the values given by the manufacturer and it meets the precision criteria given in5.1.1 to
36、5.1.3. It is also desirable that the instrument should conform to the additional performance requirements given in5.1.4. 5.1.1 Minimum precision (see A.1) Calculate the standard deviation of10measurements of the absorbance of the most concentrated calibration solution. The standard deviation shall n
37、ot exceed1,5% of the mean absorbance of this solution. Calculate the standard deviation of10measurements of the absorbance of the least concentrated calibration solution (excluding the zero member). The standard deviation shall not exceed0,5% of the mean absorbance of the most concentrated calibrati
38、on solution. 5.1.2 Limit of detection (see A.2) This is defined as twice the standard deviation of10 measurements of the absorbance of a solution containing the appropriate element at a concentration level selected to give an absorbance just above that of the zero member. The limit of detection of m
39、anganese in a matrix similar to the final test portion solution shall be less than0,024g of Mn per millilitre. 5.1.3 Graph linearity (see A.3) The value of the slope of the calibration graph covering the top20% of the concentration range (expressed as a change in absorbance) shall not be less than0,
40、7times the value of the slope for the bottom 20% of the concentration range (expressed as a change in absorbance) determined in the same way. For instruments with automatic calibration using two or more standards, it shall be established prior to the analysis, by obtaining absorbance readings, that
41、the above requirements for graph linearity are fulfilled. 5.1.4 Characteristic concentration (see A.4) The characteristic concentration of manganese in a matrix similar to the final test portion solution shall be better than0,14g of Mn per millilitre. 5.2 Ancillary equipment A strip chart recorder a
42、nd/or digital readout device is recommended to evaluate the criteria in5.1.1 to5.1.3 and for all subsequent measurements. Scale expansion can be used until the noise observed is greater than the read-out error and is always recommended for absorbances below0,1. If scale expansion has to be used and
43、the instrument does not have the means to read the value of the scale expansion factor, the value can be calculated by measuring the absorbances of a suitable solution with and without scale expansion and using the ratio of the signals obtained. 6 Sampling Carry out sampling in accordance with ISO37
44、7-2 or appropriate national standards for steel and iron. 7 Procedure WARNING Perchloric acid vapour may cause explosions in the presence of ammonia, nitrous fumes or organic matter in general. All evaporations must be carried out in fume cupboards suitable for use with perchloric acid. Ensure that
45、the spray system and drainage system are washed free from perchloric acid after use. 7.1 Test portion Weigh, to the nearest1mg, approximately1,0g of the test sample. 7.2 Blank test In parallel with the determination and following the same procedure, carry out a blank test using the same quantities o
46、f all the reagents, including the pure iron (4.1). 7.3 Determination 7.3.1 Preparation of the test solution Place the test portion (7.1) in a250ml beaker. Add20ml of hydrochloric acid (4.2), cover the beaker with a watch glass and heat gently until solvent action ceases. Add5ml of nitric acid (4.4),
47、 and boil for 1min to remove oxides of nitrogen. Add15ml of perchloric acid (4.5), and heat strongly without a cover until fuming commences. Cover with a watch glass and continue heating at a temperature at which a steady reflux of white perchloric acid fumes is maintained on the walls of the beaker
48、. Continue heating until there are no perchloric acid fumes visible inside the beaker. For samples not readily soluble in hydrochloric acid and nitric acid, add2ml of hydrofluoric acid (4.3) before the addition of15ml of perchloric acid and continue as described above.ENISO10700:1995 BSI 01-2000 5 7
49、.3.2 Treatment of the solution 7.3.2.1 Manganese contents up to 0,10% (m/m) Allow to cool, add25ml of water and heat gently to dissolve the salts. Cool again and transfer quantitatively to a250ml one-mark volumetric flask. Dilute to the mark with water and mix. Filter by decantation through a dry, medium-texture filter paper to remove any residue or precipitate, and collect the filtrate in a dry beaker after discarding the first portions. The filtrate is the test solution for determining manganese contents up to0,10% (
