BS-6200-3.18.2-1985 ISO-629-1982.pdf
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1、BRITISH STANDARD BS 6200-3.18.2: 1985 ISO 629:1982 Sampling and analysis of iron, steel and other ferrous metals Part 3: Methods of analysis Section 3.18 Determination of manganese Subsection 3.18.2 Steel: spectrophotometric method ISO title: Steel and cast iron Determination of manganese content Sp
2、ectrophotometric method UDC 669.1:543.42.062:546.711 Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:55:38 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6200-3.18.2:1985 This British Standard, having been prepared under the direction of the Iron and Steel Standards Committee, was published
3、 under the authority of the Board of BSI and comes into effect on 28 February 1985 BSI 11-1999 The following BSI references relate to the work on this standard: Committee reference ISM/18 Draft for approval 84/39008 ISBN 0 580 14266 3 National foreword This Subsection of BS 6200 has been prepared un
4、der the direction of the Iron and Steel Standards Committee. It is identical with ISO 629:1982 “Steel and cast iron Determination of manganese content Spectrophotometric method” published by the International Organization for Standardization (ISO) and supersedes method 2 for the determination of man
5、ganese in BSI Handbook No. 19. Terminology and conventions. The text of the International Standard has been approved as suitable for publication as a British Standard without deviation. Some terminology and certain conventions are not identical with those used in British Standards; attention is draw
6、n especially to the following. The comma has been used as a decimal marker. In British Standards it is current practice to use a full point on the baseline as the decimal marker. Wherever the words “International Standard” appear, referring to this standard, they should be read as “British Standard”
7、. Cross-reference. The Technical Committee has reviewed the provisions of ISO/R 377, to which reference is made in the text, and has decided that they are acceptable for use in conjunction with this standard. At present there is no corresponding British Standard for ISO 377-2, which is still at draf
8、t stage, but a related standard to ISO/R 377 is BS 1837 “Methods for the sampling of iron, steel, permanent magnet alloys and ferro-alloys”. Appropriate procedures from ISO 377-2 will be incorporated in BS 6200-2 “Methods of sampling and sample preparation”, which will be published in due course and
9、 which will supersede BS 1837. 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. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of
10、 pages This document comprises a front cover, an inside front cover, pages i and ii, pages 1 to 4, an inside back cover and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front co
11、ver. Amendments issued since publication Amd. No.Date of issueComments Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:55:38 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6200-3.18.2:1985 BSI 11-1999i Contents Page National forewordInside front cover 1Scope and field of application1 2Refer
12、ence1 3Principle1 4Reagents1 5Apparatus1 6Sampling1 7Procedure1 8Expression of results4 9Test report4 Table 1 Dilution guide for test solution3 Table 2 Preparation guide for reference solution of manganese less than 0,05 % (m/m)3 Table 3 Preparation guide for reference solution of manganese between
13、0,050 and 4 % (m/m)3 Publication referred toInside back cover Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:55:38 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ii blank Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:55:38 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6200-3.18.2:
14、1985 BSI 11-19991 1 Scope and field of application This International Standard specifies a spectrophotometric method for the determination of manganese in steel and cast iron. The method is applicable to products having manganese contents between 0,001 and 4 % (m/m). 2 Reference ISO 377-2, Selection
15、 and preparation of samples and test pieces of wrought steels Part 2: Samples and test pieces in-tended for the determination of the chemical composition1). 3 Principle Dissolution of a test portion in sulphuric-phosphoric acid mixture and nitric acid. Treatment of the test solution with perchloric
16、acid. Formation of the permanganate ion by sodium periodate. Spectrophotometric measurement of the test solution at wavelength of about 545 nm. 4 Reagents During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only distilled water or water of equivalent pu
17、rity. NOTEVerify by blank tests that relevant reagents are free from manganese. Wherever necessary, the results should be corrected accordingly. 4.1 Water, free from organic matter. Bring to the boil water acidified with 10 ml/l of sulphuric acid ( about 1,83 g/ml), add several crystals of sodium pe
18、riodate (NaIO4) and keep boiling for 10 min. 4.2 Pure iron, free from manganese. 4.3 Hydrochloric acid, about 1,19 g/ml. 4.4 Nitric acid, about 1,40 g/ml. 4.5 Perchloric acid, about 1,67 g/ml. NOTEIt is also possible to use perchloric acid, about 1,54 g/ml. 127 ml of perchloric acid, about 1,54 g/ml
19、 is equivalent to 100 ml of perchloric acid, about 1,67 g/ml. 4.6 Perchloric acid, diluted 1 + 499. 4.7 Sulphuric/phosphoric acid mixture To 600 ml of water add in the following order, carefully and stirring at the same time, 100 ml of sulphuric acid ( about 1,83 g/ml) and 150 ml of phosphoric acid
20、( about 1,71 g/ml). Cool and dilute to 1 000 ml with water. 4.8 Sodium periodate, 50 g/l solution. 4.9 Manganese, standard solution 4.9.1 Stock solution Weigh, to the nearest 0,001 g, 2,877 g of potassium permanganate, dissolve in 500 ml of water and add 10 ml sulphuric acid ( about 1,83 g/ml). Deco
21、lorize the solution with hydrogen peroxide about 30 % (m/m) or with a stream of sulphur dioxide. In the latter case, eliminate the excess of reagent by boiling. After cooling, transfer the solution to a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix. 1 ml of this stock sol
22、ution contains 1,00 mg of Mn. 4.9.2 Standard solution A Transfer 100 ml of the stock solution (4.9.1) to a 1 000 ml one-mark volumetric flask and dilute to the mark with water and mix. 1 ml of standard solution A contains 0,1 mg of Mn. 4.9.3 Standard solution B Transfer 250 ml of the standard soluti
23、on A (4.9.2) to a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix. 1 ml of standard solution B contains 0,025 mg of Mn. 5 Apparatus Ordinary laboratory apparatus and 5.1 Spectrophotometer 6 Sampling Sampling shall be carried out in accordance with ISO 377-2 or appropriate n
24、ational standards for cast iron. 7 Procedure WARNING: Perchloric acid vapour may cause explosions in the presence of ammonia, nitrous fumes or organic material in general. 7.1 Test portion According to the presumed manganese content, weigh, to the nearest 0,001 g, the following mass (m) of the test
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