EN 24946:1990
(Main)Determination of copper content in steel and cast iron
Determination of copper content in steel and cast iron
This method is applicable to copper contents between 0.02 % (m/m) and 5 % (m/m). Specifies principle, reagents, apparatus, sampling, procedure, expression of results and test report. Annex A gives additional information on the international co-operative tests. Annex B includes the graphical representation of precision data.
Ermittlung des Kupfergehalts von Stahl und Roheisen
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Dosage du cuivre dans les aciers et les fontes
La présente Norme internationale spécifie une méthode spec- trophotométrique au 2,2'-biquinolyle, de dosage du cuivre dans les aciers et les fontes. La méthode est applicable aux teneurs en cuivre comprises entre 0,02 et 5 % (m/m).
Določevanje bakra v jeklu in litem železu
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Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Ermittlung des Kupfergehalts von Stahl und RoheisenDosage du cuivre dans les aciers et les fontesDetermination of copper content in steel and cast iron77.080.01Železne kovine na splošnoFerrous metals in generalICS:Ta slovenski standard je istoveten z:EN 24946:1990SIST EN 24946:1997en01-december-1997SIST EN 24946:1997SLOVENSKI
STANDARD
International Standard INTERNATIONAL ORGANIZATION FOR STANDARDIZATION~MEIK~YHAPO~HAFI OPI-AHM3ALlMR I-IO CTAHAAPTbl3AIJWl~ORGANlSATlON INTERNATIONALE DE NORMALISATION Steel and cast iron - Determination of copper content - 2,2’-Diquinolyl spectrophotometric ‘method Aciers et fontes - Dosage du cuivre - M&ode spectrophotom&ique au 2,2’-biquinolyle First edition - 1984-12-15 Corrected and reprinted 1986-12-15 UDC 669.131.14 : 543.42 : 546.56 Ref. No. IS0 4946-1984 1 E) Descriptors : steels, cast iron, chemical analysis, determination of content, copper, spectrophotometric analysis. Price based on 6 pages SIST EN 24946:1997
Foreword IS0 (the International Organization for Standardization) is a worldwide federation of national standards bodies (IS0 member bodies). The work of preparing International Standards is normally carried out through IS0 technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, govern- mental and non-governmental, in liaison with ISO, also take part in the work. Draft International Standards adopted by the technical committees are circulated to the member bodies for approval before their acceptance as International Standards by the IS0 Council. They are approved in accordance with IS0 procedures requiring at least 75 % approval by the member bodies voting. International Standard IS0 4946 was prepared by Technical Committee ISO/TC 17, S tee/. 0 International Organization for Standardization, 1984 Printed in Switzerland SIST EN 24946:1997
INTERNATIONAL STANDARD IS0 4946-1984 (E) Steel and cast iron - Determination of copper content - 2,2’-Diquinolyl spectrophotometric method 1 Scope and field of application This International Standard specifies a 2,2’-diquinolyl spec- trophotometric method for the determination of copper in steel and cast iron. The method is applicable to copper contents between 0,02 and 5 % (m/m). 2 Reference ISO/R 377, Selection and preparation of samples and test pieces for wrought steel. 3 Principle Dissolution of a test portion with appropriate acids. Fuming with perchloric acid to remove hydrochloric and nitric acids and dehydrate silicic acid. Reduction of copper to copper(l) in hydrochloric acid solution by means of ascorbic acid. Formation of a coloured compound of copper-( I) with 2,2’-diquinolyl. Spectrophotometric measurement at a 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 purity, free from copper. 4.1 High-purity iron, containing 0,001 % (m/m) or less of copper. 4.2 Hydrochloric acid, Q approximately I,19 g/ml. 4.3 Nitric acid, e approximately 1,40 g/ml. 4.4 Perchloric acid, Q approximately 1,54 g/ml. NOTE - Perchloric acid, Q approximately I,67 g/ml, may also be used. 100 ml of perchloric acid, Q approximately I,54 g/ml, is equivalent to 79 ml of perchloric acid, Q approximately I,67 g/ml. 4.5 Perchloric acid, Q approximately I,54 g/ml, diluted 1 + 7. 4.6 Dimethylformamide (N, IV-dimethylformamide), Q approximately 0,944 g/ml. 4.7 Ascorbic acid, 200 g/l solution. Dissolve 20 g of ascorbic acid in water, dilute to 100 ml and mix. Prepare this solution immediately before use. 4.8 2,2’-Diquinolyl, solution. Dissolve 0,60 g of 2,2’-diquinolyl (cuproine) in the dimethyl- formamide (4.61, dilute to 1 litre with the same dimethyl- formamide and mix. Keep this solution in a dark-coloured glass receptacle and pro- tected from the light. 4.9 Copper, standard solutions. 4.9.1 Copper, standard solution, corresponding to I,0 g of Cu per litre. Weigh, to the nearest 0,000 1 g, 1,000 0 g of high purity cop- per and dissolve in a minimum of the nitric acid (4.3). Heat to boiling to remove nitrous fumes. Cool and transfer the solution quantitatively to a 1 000 ml one-mark volumetric flask, dilute to the mark and mix. 1 ml of this standard solution contains 1 mg of Cu. 4.9.2 Copper, standard solution, corresponding to 0,050 g of Cu per litre. Transfer 50,O ml of the copper standard so 1 000 ml one-mark volumetric flask, dilute to 1 ml of this standard solution contains 0,05 ution (4.9.1) to a the mark and mix. mg of Cu. 5 Apparatus Ordinary laboratory apparatus and 5. I Spectrophotometer. SIST EN 24946:1997
IS0 49464984 (El 6 Sampling Table 1 Carry out sampling in accordance with ISO/R 377 or ap- propriate national standards for cast iron. Copper content Volume of test solution (7.3.1) Volume of aliquot portion % h/m) ml ml 0,02 to 0,3 100 10 0,3 to 0,6 100 5 0,6 to I,5 250 5 I,5 to 5,0 500 5 7 Procedure WARNING Transfer the selected aliquot portion to a 50 ml one-mark volumetric flask. If the aliquot portion is 5 ml, add 5 ml of the perchloric acid (4.5). a) Perchloric acid vapour may cause explosions in the presence of ammonia, nitrous fumes or organic material in general. Add, in the following order, shaking after each addition : b) Dimethylformamide is a hazardous substance and should not be handled by pregnant women. It should be handled with safety gloves in a fume hood. - 5 ml of the ascorbic acid solution (4.7) ; - 25 ml of the 2,2’-diquinolyl solution (4.8). 7.1 Test portion Dilute to the mark and mix. Cool for 5 min in a water-bath at about 20 OC. Weigh, to the nearest 0,001 g, approximately 0,5 g (m) of the test sample. Finally, readjust to volume and mix again. 7.3.3 Preparation of the compensating solution 7.2 Blank test Transfer an aliquot portion of the test solution (7.3.1) similar to the aliquot portion for the development of the colour (7.3.2) to a 50 ml one-mark volumetric flask. Add, in the following order, shaking after each addition : - 5 ml of the ascorbic acid solution (4.7); 7.3 Determination - 25 ml of the dimethylformamide (4.6). Dilute to the mark and mix. Cool for 5 min in a water-bath at about 20 OC. 7.3.1 Preparation of the test solution Introduce the test portion (7.1) into a 250 ml beaker. Add 10 ml of the hydrochloric acid (4.2) and 5 ml of the nitric acid (4.3), cover the beaker with a watch-glass and heat until solvent action ceases. Finally, readjust to volume and mix again. 7.3.4 Spectrophotometric measurement Carry out the spectrophotometric measurement of the test solution at a wavelength of about 545 nm, in a cell of 2 cm optical path length, after having adjusted the spectrophoto- meter (5.1) to zero absorbance in relation to the compensating solution (7.3.3). NOTE - For samples of high chromium content, dissolve first in the hydrochloric acid (4.2) and when all effervescence has ceased oxidize by adding the nitric acid (4.31, drop by drop. Add IO ml of the perchloric acid (4.4) and evaporate to fuming. Continue fuming for 3 min. NOTE - For copper contents below 0,06 % (~nlm), 4 cm cells may be used if the sensitivity of the spectrophotometer is not sufficient with 2 cm cells. Cool,
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