SIST EN 24829-2:1998
(Main)Steel and cast iron - Determination of total silicon content - Reduced molybdosilicate spectrophotometric method - Part 2: Silicon content between 0,01 and 0,05% (ISO 4829-2:1988)
Steel and cast iron - Determination of total silicon content - Reduced molybdosilicate spectrophotometric method - Part 2: Silicon content between 0,01 and 0,05% (ISO 4829-2:1988)
Quality. Rationalization.
Eisen und Stahl - Ermittlung des Gesamtsiliziumgehaltes - Spektrophotometrisches Verfahren (Reduzierte Molybdosilicate) Teil 2: Siliziumgehalte zwischen 0,01 und 0,05% (ISO 4829-2:1988)
Qualitaet. Rationalisierung.
Aciers et fontes - Détermination de la teneur en silicium total - Méthode spectrophotométrique par molybdosilicate réduit - Partie 2: Teneur en silicium entre 0,01 et 0,05% (ISO 4829-2:1988)
Qualité. Rationalisation.
Jeklo in lito železo - Določanje celotnega silicija - Spektrofotometrijska metoda (z reduciranim molibdo-silikatom) - 2. del: Deleži silicija 0,01 do 0,05 % (ISO 4829-2:1988)
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Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Eisen und Stahl - Ermittlung des Gesamtsiliziumgehaltes - Spektrophotometrisches Verfahren (Reduzierte Molybdosilicate) Teil 2: Siliziumgehalte zwischen 0,01 und 0,05% (ISO 4829-2:1988)Aciers et fontes - Détermination de la teneur en silicium total - Méthode spectrophotométrique par molybdosilicate réduit - Partie 2: Teneur en silicium entre 0,01 et 0,05% (ISO 4829-2:1988)Steel and cast iron - Determination of total silicon content - Reduced molybdosilicate spectrophotometric method - Part 2: Silicon content between 0,01 and 0,05% (ISO 4829-2:1988)77.080.01Železne kovine na splošnoFerrous metals in general77.040.30Kemijska analiza kovinChemical analysis of metalsICS:Ta slovenski standard je istoveten z:EN 24829-2:1990SIST EN 24829-2:1998en01-avgust-1998SIST EN 24829-2:1998SLOVENSKI
STANDARD
SIST EN 24829-2:1998
SIST EN 24829-2:1998
SIST EN 24829-2:1998
INTERNATIONAL STANDARD INTERNATIONAL ORGANIZATION FOR STANDARDIZATION ORGANISATION INTERNATIONALE DE NORMALISATION ME>KfiYHAPOflHAR OPI-AHM3A~Mfl l-l0 CTAHfiAPTM3A~MM Steel and iron - Determination of total Silicon content - Reduced molybdosilicate spectrophotometric method - Part 2: Silicon contents between 0,Ol and 0,05 % Aciers et forltes - Dosage du silicium total - Methode spectrophotomhtrique au molybdosilica te rhduit - Partie 2: Teneurs en silicium comprises entre O,Ol et 0,05 % ISO 4829-2 First edition 1988-12-01 Reference number ISO 4829-2 : 1988 (E) SIST EN 24829-2:1998
ISO 4829-2 : 1988 (El Foreword ISO (the International Organization for Standardization) is a worldwide federation of national Standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Esch 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. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization 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. They are approved in accordance with ISO procedures requiring at least 75 % approval by the member bodies voting. International Standard ISO 4829-2 was prepared by Technical Committee ISO/TC 17, S teeL Users should note that all International Standards undergo revision from time to time and that any reference made herein to any other International Standard implies its latest edition, unless otherwise stated. ISO 4829 consists of the following Parts, under the general title Steel and iron - Determination o f total silicon con ten t - Reduced molybdosilica te spec tropho tome tric method: - Part 1: Silicon contents between 0,05 and 1,O % - Part 2: Silicon contents between 0,Ol and 0,05 % 0 International Organkation for Standardkation, 1988 Printed in Switzerland SIST EN 24829-2:1998
INTERNATIONAL STANDARD ISO 4829-2 : 1988 (E) Steel and iron - Determination of total Silicon content - Reduced molybdosilicate spectrophotometric method - Part 2: Silicon contents between 0,Ol and 0,05 941 1 Scope and field of application This International Standard specifies a spectrophotometric method using reduced molybdosilicate for the determination of total Silicon in steel and iron. The method is applicable to Silicon contents between 0,Ol and 0,05 % (mlm) in steel and iron. 2 References ISO 377, Wrought steel - Selection and preparation of samples and test pieces. ISO 385- 1, Laboratory glassware - Burettes - Part 7 : General requiremen ts. ISO 648, Laboratory glassware - One-mark pipettes. ISO 1042, Laboratory glassware - One-mark volumetric flasks . ISO 5725, Precision of test methods - Determination of repeatability and reproducibility for a Standard test method b y in ter-labora tory tes ts . 4 Reagents During the analysis, unless otherwise stated, use only reagents of recognized analytical grade. Reagents supplied in glass bottles, once opened, may absorb moisture and become reactive to glassware. Alkaline reagents, e.g. sodium carbonate and sodium Peroxide, are particularly susceptible. To avoid the risk of significant contamination arising from this Source, it is recommended that only freshly opened bottles of all reagents be used for the preparation of reagent solutions. In addition, only water prepared by distillation shall be used for the preparation of reagent solutions and throughout the pro- cedure. Water demineralized by ion-exchange shall not be used as it may contain significant amounts of colloidal silica. To avoid adventitious contamination, the water shall be prepared, as required, for the specific purpose, and collected in polypropylene Containers for immediate use. All solutions shall be freshly prepared and stored in polypropylene or polytetrafluoroethylene Containers. 4.1 Pure iron, Silicon content less than 2 pg/g. 3 Principle Dissolution of a test Portion in a hydrochloric acid/nitric acid mixture. Fusion of the acid-insouble residue with sodium Peroxide. Formation of the oxidized molybdosilicate (yellow) complex in weak acid Solution. Selective reduction of the molybdosilicate complex to a blue complex with ascorbic acid, after increasing the sulfuric acid concentration and adding oxalic acid to prevent the interference of phosphorus, arsenic and vanadium. Spectrophotometric measurement of the reduced blue complex at a wavelength of about 810 nm. 4.2 Sodium Peroxide, particle size of minus 500 Pm. 4.3 Sulfuric acid, diluted 1 + 3. To 600 ml of water add cautiously, with stirring, 250 ml of sulfuric acid, Q about 1,84 g/ml. Cool, dilute to 1 000 ml and mix. 4.4 Sulfuric acid, diluted 1 + 19. To 800 ml of water add cautiously, with stirring, 50 ml of sulfuric acid, Q about 1,84 g/ml. Cool, dilute to 1 000 ml and mix. 1 SIST EN 24829-2:1998
ISO 4829-2 : 1988 (El 4.5 Hydrochlorit acid/nitric acid mixture. 5 Apparatus Add 180 ml of hydrochloric acid, Q about 1,19 g/ml, and 65 ml of nitric acid, Q about 1,40 g/ml, to 500 ml of water. Cool, dilute to 1 000 ml and mix. Ordinary laboratory apparatus and 5.1 Beakers ethylene. and lids, of polypropylene or polytetrafluoro- 4.6 Ascorbic acid, 20 g/l Solution. 5.2 Crucibles, of zirconium metal, of 50 ml capacity. Prepare this Solution immediately before use. 4.7 Oxalic acid, solution. Dissolve 5 g of oxalic acid dihydrate (C2HZ04m2H20) in water, dilute to 100 ml and mix. 48 . Hydrogen Peroxide, Solution. Dilute 200 ml of hydrogen Peroxide, 300 g/l, to 1 000 ml and mix. 4.9 Potassium permanganate, 22,5 g/l Solution. Filter before use. 4.10 Sodium molybdate, solution. Dissolve 2,5 g of sodium molybdate dihydrate (Na2Mo04.2HZO) in 50 ml of water and filter through a medium-texture filter Paper. Immediately before use, add 15 ml of sulfuric acid (4.41, dilute to 100 ml and mix. 4.11 Silicon, Standard Solution. 4.11.1 Silicon stock Solution, containing 1 g of Si per litre. Weigh, to the nearest 0,l mg, 2,139 3 g of freshly calcined high-purity silica ( > 99,9 % Si02) and transfer to a platinum crucible. (The high-purity silica shall be calcined for 1 h at 1 100 OC and cooled in a desiccator immediately before use.) Mix thoroughly with 16 g of anhydrous sodium carbonate and fuse at 1 050 OC for 30 min. Extract the fusion product with 100 ml of water in a polypropylene or polytetrafluoroethylene beaker (see the note). Transfer the extract, which should con- tain no trace of residue, to a 1 000 ml one-mark volumetric flask, dilute to the mark and mix. Transfer immediately to a weil-stoppered polytetrafluoroethylene bottle for storage. 1 ml of this stock Solution contains 1 mg of Si. NOTE - Extraction of the fusion product may require gentle heating. 4.11.2 Silicon Standard Solution, containing 20 mg of Si per litre. Transfer IO,0 ml of Silicon stock Solution (4.11 .l) to a 500 ml one-mark volumetric flask. Dilute to the mark and mix. Transfer immediately to a weil-stoppered polytetrafluoroethylene bottle for immediate use. 1 ml of this Standard Solution contains 20 ug of Si. NOTE - Vitreous carbon zirconium metal crucibles. crucibles may be used as alternatives to 5.3 Volumetric glassware. All volumetric glassware shall be class A, in accordance with ISO 385-1, ISO 648 or ISO 1042, as appropriate. The u se of glassware sha II be restricted to a minimum of con- tact ti me and borosilicate glass shall be used as far as possible. 5.4 Spectrophotometer. The spectrophotometer shall be equipped to measure absorb- ante with a spectral band width of 10 nm or less at a wavelength of 810 nm. Wavelength measurement shall be accurate to f: 2 nm, as measured by the absorption maximum of a didymium filter at 803 nm, or other suitable calibration method. The absorption measurement for the Solution of maxi- mum absorbance shall have a repeatability, expressed as a relative deviation, of + 0,3 % or better. 6 Sampling Carry ou t sampling in accordance with ISO 377 or appropriate national Standards for iron. 7 Procedure 7.1 Test Portion Weigh, to the nearest 1 mg, 0,50 $r 0,Ol g (m) of test Sample in the form of fine Chips, turnings, millings or filings. 7.2 Blank test In parallel with the determination and following the same pro- cedure, carry out two blank tests using the same quantities of all the reagents but using 0,50 &- 0,Ol g of pure iron (4.1) in- stead of the test Portion. lt is essential that blank values be controlled at consistently low and reproducible values. lt is recommended that duplicate blanks be run with each batch of tests and the mean value be used as the basis for calculation. High or divergent blank values should be considered unacceptable and Steps should be taken to trace the Source of contamination by checking the quality of the water and of individual reagents before proceeding further. In particular, sodium peroxide and potassium permanganate req
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