SIST EN 24934:1997
(Main)Steel and cast iron - Determination of sulphur content - Gravimetric method (ISO 4934:1980, ed. 1)
Steel and cast iron - Determination of sulphur content - Gravimetric method (ISO 4934:1980, ed. 1)
Stahl und Gußeisen - Ermittlung des Schwefelgehalts - Gravimetrisches Verfahren (ISO 4934:1980, Ausg. 1)
Aciers et fontes - Dosage de soufre - Méthode gravimétrique (ISO 4934:1980, éd. 1)
Jeklo in lito železo - Določevanje žvepla - Gravimetrična metoda (ISO 4934:1980)
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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Stahl und Gußeisen - Ermittlung des Schwefelgehalts - Gravimetrisches Verfahren (ISO 4934:1980, Ausg. 1)Aciers et fontes - Dosage de soufre - Méthode gravimétrique (ISO 4934:1980, éd. 1)Steel and cast iron - Determination of sulphur content - Gravimetric method (ISO 4934:1980, ed. 1)77.080.01Železne kovine na splošnoFerrous metals in general77.040.30Kemijska analiza kovinChemical analysis of metalsICS:Ta slovenski standard je istoveten z:EN 24934:1989SIST EN 24934:1997en01-december-1997SIST EN 24934:1997SLOVENSKI
STANDARD
SIST EN 24934:1997
SIST EN 24934:1997
SIST EN 24934:1997
International Standard INTERNATIONAL ORGANIZATION FOR STANDARDIZATION@MEIK,lV’HAPOflHAR OPrAHM3AlWlR fl0 CTAH~APTbl3Al@lWORGANISATION INTERNATIONALE DE NORMALISATION Steel and cast iron - Determination of sulphur content - Gravimetric method Aciers et fontes - Dosage du soufre - Methode gravimktrique First edition - 1980-10-01 UDC 669.13/.14 : 543.21 : 546.22 Ref. No. ISO 4934-1980 (E) Descriptors : steels, cast iron, Chemical analysis, determination of content, sulphur, gravimetric method. Price based on 5 pages SIST EN 24934:1997
Foreword ISO (the International Organization for Standardization) is a worldwide federation of national Standards institutes WO member bedies). The work of developing Inter- national Standards is carried out through ISO technical committees. Every member body interested in a subject for which a technical committee has been set up has the right to be represented on that committee. International organizations, governmental 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 ISO Council. International Standard ISO 4934 was developed by Technical Committee ISO/TC 17, Ree/, and was circulated to the member bodies in October 1978. lt has been approved by the member bodies of the following countries : Austria Belgium Bulgaria Czechoslovakia Denmark Egypt, Arab Rep. of Finland Germany, F. R. Hungary The member bodies of the on technical grounds : India Iran Italy Japan Korea, Dem. P. Rep. of Korea, Rep. of New Zealand Norway Poland following cou ntries expressed Canada 0 International Organkation for Standardkation, 1980 Printed in Switzerland Romania South Africa, Rep. of Sweden Switzerland Turkey United Kingdom USA USSR Y ugoslavia pproval of the document 1 I I I l 1 I l I l I l / SIST EN 24934:1997
INTERNATIONAL STANDARD ISO 49344980 (El Steel and cast iron - Determination of sulph Gravimetric method 1 Scope and field of application This International Standard specifies a gravimetric method for the determination of the sulphur content of steels and cast iron, excluding steels containing selenium. The method is particu- larly suitable as a reference method for the standardization of samples on which certified Standard values are to be estab- lished. The method is applicable to products having sulphur contents greater than 0,003 % (mlm). 2 References ISOIR 377, Selection and preparation of samples and fest pieces for wrought steel. 1) ISO 565, Test sieves - Wo ven me tal wire clo th and perfora ted plate - Nominal sizes of apertures. 3 Principle Dissolution of a test Portion in dilute nitric acid in the presence of bromine, or in dilute nitric acid and concentrated hydrochloric acid in the presence of bromine (with the aid of an appropriate device to prevent sulphur losses). Addition of hydrofluoric acid and perchloric acid and evaporation of the solution until white fumes of perchloric acid are evolved. If necessary, volatilization of chromium as chromyl chloride. Chromatographie Separation of the sulphate ions in an alumina column and elution with ammonium hydroxide solution. Precipitation of the sulphate ions as barium sulphate under carefully controlled conditions and filtering, washing, heating and weighing. 4 Reagents During the analysis, use only reagents of recognized analytical grade and distilled water or water of equivalent purity. 4.1 Aluminium Oxide (alumina), prepared for chromatography, of particle size corresponding to a sieve mesh size of 75 to 150 Pm (supplementary series R 40/3 of ISO 565). Alumina designated alkaline, neutral or acid may be used. Place about 200 g of the dry alumina in a 400 ml beaker con- taining 300 ml of water and place the beaker in a sink. Insert a glass tube having a bore of 5 mm, such that it extends to the bottom of the beaker and connect the tube to a water supply. Adjust the water flow so that the suspended fine material overflows the rim of the beaker. Continue this treatment until all the fine material, which does not settle within 1 min of stop- ping the water flow, is removed. Pour off the supernatant liquid from the coarser material, add the hydrochloric acid (4.4) in an amount sufficient to cover the alumina, stir and allow to stand for not less than 12 h. Pour off the hydrochloric acid and wash the alumina with water as described in the second Paragraph. For preparation of the column, make a slurry of the washed alumina and the hydrochloric acid Solution (4.8). 4.2 Bromine. 4.3 Nitrit acid, Q approximately 1,40 g/ml. 4.4 Nitrit acid, 1 + 1 dilution. 4.5 Hydrochlorit acid, Q approximately l,l9 g/ml. 4.6 Hydrochlorit acid, 1 + 1 dilution. 4.7 Hydrochlorit acid, 1 + 9 dilution. 4.8 Hydrochlorit acid, 1 + 19 dilution. 4.9 Perchlorit acid, Q approximately 154 g/ml. NOTE - If this reagent is shown to have a high sulphate content, this may be removed by passing the reagent through the adsorption column (5.3). 4.10 Perchlorit acid, 1 + 98 dilution. 4.11 Hydrofluoric acid, Q approximately 1,14 g/ml. 4.12 Ammonium hydroxide, Q approximately 0,90 g/mI. 1) Under revision. SIST EN 24934:1997
ISO 49344980 (E) 4.13 Ammonium hydroxide, 1 + 19 dilution. if contact is not maintained with the alumina column. Ensure that all alumina particles are removed from the column sides above the top plug. 4.14 Ammonium hydroxide, 1 + 99 dilution. Add some of the hydrochloric acid Solution (4.8) to the reser- voir, and adjust the flow rate to 10 to 15 ml per minute. If the flow cannot be adjusted to this rate, empty the column and repeat the preparation. 4.15 Iron(ll) perchlorate solution. Transfer 5 g of high purity iron of very low sulphur content to a 500 ml narrow-necked conical flask, and dissolve in a mixture of 25 ml of the perchloric acid (4.9) and 375 ml of water by heating in a water bath at 50 OC. Pass by suction 20 ml of water through the column and follow with 20 ml of the ammonium hydroxide Solution (4.13) and then 20 ml of water. Combine the last two eluates and test for absence of aluminium salts by adjusting the pH of the solution until faintly ammoniacal. If aluminium hydroxide precipitates on standing, pass 20 ml of the hydrochloric acid Solution (4.7) and then 20 ml of water through the column. Repeat the treatment with 20 ml of the ammonium hydroxide Solution (4.13) and 20 ml of water, testing the ammoniacal eluates for absence of aluminium salts as before. When about two-thirds of the flask from the water bath and iron has d allow it to issolved, cool. remove the Close the flask with a rubber stopper provided with a one-way valve to permit the escape of gases without the ingress of air. 4.16 Sulphuric acid, solu tion imately 48 mg of sulphur per Iitre. corresponding to approx- If aluminium hydroxide still precipitates, pass some of the hydrochloric acid Solution (4.6) through the column for 1 h without suction and then wash with 50 ml of water. Pass 20 ml of the ammonium hydroxide Solution (4.13) and 20 ml of water Add 2,8 ml of sulphuric acid, Q approximately 184 g/ml, to ab.out 500 ml of water. Dilute to 1 000 ml and mix. Take 30 ml of this Solution, dilute to 1 000 ml and mix. through the column aluminium sa Its. and test these eluates for absence of 4.17 Barium chloride dihydrate, 122 g/l Solution. Repeat this sequence of washing until there is no evidente of aluminium salts being eluted from the column. Finally, wash with 30 ml of the hydrochloric acid Solution (4.8). Dissolve 122 g of barium chloride dihydrate (BaC12.2H20) in water, dilute to 1 000 ml and mix. Filter this Solution through Paper V just before use. a non-hardened, texture filter When the tube is not in use, immerse and fit a rubber bung to the reservoir. the lower part in water 1 ml of sulphur this solution is equ to aPP roximatel yO,16 mg of 6 Sampling 4.18 Methyl orange, 0,50 g/l solution. Select and prepare the samples as specified in ISO/R 377. 7 Procedure 5 Apparatus Normal laboratory apparatus, and 7.1 Test Portion Take a test Portion tent as follows : according to the anticipated sulphur con- 5.1 Conical flask, of capacity 1 000 ml, having a ground- glass neck. a) for sulphur contents up to 0,005 % (mlm), weigh, to the nearest 0,001 g, two test portions, each of approx- imately 10 g; 5.2 Allihn condenser (four or six bulb type). 53 . Adsorption column (see the figure). b) for sulphur contents of 0,005 % up to 0,05 % (mlm), weigh, to the nearest 0,001 g, a test Portion of approx- imately 10 g; Prepare the adsorption column as follows. Fit the column tube into a one-hole rubber bung just below the reservoir to act as a gasket for fixing the tube in a suction filtra- tion flask. Fit the tube into the suction flask and place a well- packed plug of quartz wool, about 20 mm thick, in the narrow end of the tube. Transfer sufficient alumina slurry (4.1) into the tube to make a column 100 to 120 mm long. Using the hydrochloric acid Solution (4.8
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