EN 24501:1993

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Hardmetals - Determination of titanium - Photometric peroxide method (ISO 4501:1978)Hartmetalle - Bestimmung des Titangehaltes - Photometrisches Wasserstoffsuperoxidverfahren (ISO 4501:1978)Métaux durs - Détermination du titane - Méthode photométrique au peroxyde (ISO 4501:1978)Hardmetals - Determination of titanium - Photometric peroxide method (ISO 4501:1978)77.160Metalurgija prahovPowder metallurgyICS:Ta slovenski standard je istoveten z:EN 24501:1993SIST EN 24501:2000en01-december-2000SIST EN 24501:2000SLOVENSKI
STANDARD
INTERNATIONAL STANDARD INTERNATIONAL ORGANIZATION FOR STANDARDIZATIONWlEX,QYHAPO~HAR OPl-AHl43AUblR I-IO CTAH~APTM3AL&lM.ORGANISATION INTERNATIONALE DE NORMALISATION Hardmetals - Determination of titanium - Photometric peroxide method M&auxdurs - Determination du titane - Methode pho tombrique au peroxyde First edition - 1978-08-01 UDC 621.762 _ 661.665.2 : 546.82 : 543.42 Ref. No. ISO 4501-1978 (E) Descriptors : hardmetals, Chemical analysis, determination of content, titanium, spectrophotometric analysis. Price based on 3 pages SIST EN 24501:2000

FOREWORD ISO (the International Organization for Standardization) is a worldwide federation of national Standards institutes (ISO member bodies). The work of devcloping International 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 arc circuiated to the member bodies for approval before their acceptance as International Standards by the ISO Council. International Standard ISO 4501 was developed by Technical Committee ISO/TC 119, Powder metallurgical materials and products, and was circulated to the member bodies in June 1977. lt has been approved by the member bodies of the following countries : Australia Germany Austria I taly Bulgaria Japan Canada Mexico Czechoslovakia Poland Egypt, Arab Rep. of Romania France South Africa, Rep. of Spain Sweden Turkey United Kingdom U.S.A. U.S.S. R. Yugoslavia No member body expressed disapproval of the document. cc) International Organkation for Standardizat ion, 1978 l Printed in Switzerland SIST EN 24501:2000

--~ -~ INTERNATIONAL STANDARD ISO 4501-1978 (E) Hardmetals - Determination of titanium - Photometric peroxide method 1 SCOPE 5.7 Sulphuric acid, p 1,84 g/ml. This International Standard specifies a photometric peroxide method for the determination of the titanium content of carbides and hardmetals. 5.8 Sulphuric acid, p 1,54 g/ml (sulphuric acid, p 1,84 g/ml, diluted 1 -t 1). 5.9 Hydrogen Peroxide, 30 % (mlm). 2 FIELD OF APPLICATION This method is applicable to - carbide and binder metal powder mixtures, free of lubricant, - all grades of presintered or sintered hardmetals, with a titanium content exceeding 0,2 % (mlm). 5.10 Hydrofluoric acid, p 1 ,12 g/ml. 5.11 Nitrit acid, p 1,40 g/ml. 6 APPARATUS Ordinary laboratory apparatus and 3 PRINCIPLE 6.1 Spectrophotometer or filter Photometer. Formation of a yellow complex of pertitanic acid. Deter- mination of the absorbance of the complex. 4 INTERFERING ELEMENTS The effect of interfering elements which also form coloured complexes with hydrogen peroxide under the conditions specified, for example vanadium and molybdenum, shall be taken into account. A correction tan be applied if the content is below 5 % (mlm) of each. 7 SAMPLE PREPARATION 7.1 The Sample shall be crushed to a powder in a mortar made of a material which does not alter the Sample composition. The powder shall pass a 0,18 mm sieve. 7.2 The analysis shall be carried out on two or three test portions. 8 PROCEDURE 5 REAGENTS 8.1 Preparation During the analysis, use only reagents of recognized ana- lytical grade, and only distilled water or water of equivalent purity. Select the mass of the test Portion, the volume of the volumetric flask and the cell length in accordance with table 1. TABLE 1 5.1 Ammonium hydrogen fluoride. 5.2 Ammonium sulphate. 5.3 Sodium disulphite. 5.4 High-purity titanium metal or titanium dioxide, analysed for all impurities exceeding 0,Ol % (mlm) each. Titanium content % (mh?) 0,2 to 4 2 to 8 5to15 10t030 Test Portion mass g 02 02 02 OJ Flask volume ml 250 250 500 500 5.5 Citric acid Solution, 30 % (mlm). 5.6 Perchlorit acid, p 1,54 or 1,67 g/ml. NOTE - Approximately 17 mg of titanium in 250 ml of final Solution gives unit absorbance with a 10 mm cell. Gell length mm 20 10 10 10 1 SIST EN 24501:2000

ISO 4501-1978(E) 8.2 Test Portion Weigh, to the nearest 0,000 1 g, 0,l or 0,2 g of the test Sample. coloured and the comp lensating solu tions at a wavelength of 420 nm using the sa me cell or a matched pair of cells. 9 ELIMINATION OF INTERFERENCES 8.3 Attack 9.1 Vanadium Transfer the test Portion into a 100 to 200 ml conical flask or a 250 ml beaker. Add 5 g of the ammonium sulphate (5.2) and 10 ml of the sulphuric acid (5.7). Cover the beaker or flask with a watch glass. Heat near the boiling Point until complete dissolution is achieved. Alternative dissolution method : Transfer the test Portion into a platinum dish. Add IO ml of water and 5 ml of the hydrofluoric acid (5.10). Cover the dish with a polypropylene or platinum cover. Heat to approximately 80 “C. Add the nitric acid (5.11) dro
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