EN 24829-1:1990
(Main)Steel and cast iron - Determination of total silicon content - Reduced molybdosilicate spectrophotometric method - Part 1: Silicon content between 0,05 and 1% (ISO 4829-1:1986)
Steel and cast iron - Determination of total silicon content - Reduced molybdosilicate spectrophotometric method - Part 1: Silicon content between 0,05 and 1% (ISO 4829-1:1986)
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 represents the precision data graphically.
Eisen und Stahl - Ermittlung des Gesamtsiliziumgehaltes - Spektrophotometrisches Verfahren (Reduzierte Molybdosilicate) - Teil 1: Siliziumgehalte zwischen 0,05 und 1% (ISO 4829-1:1986)
Verstaendigung und Kommunikation. Qualitaet. Rationalisierung.
Aciers et fontes - Détermination de la teneur en silicium total - Méthode spectrophotométrique par molybdosilicate réduit - Partie 1: Teneur en silicum entre 0,05 et 1% (ISO 4829-1:1986)
La présente Norme internationale spécifie une méthode spectrophotométrique au molybdosilicate réduit pour le dosage du silicium total dans les aciers et les fontes. La méthode est applicable aux teneurs en silicium comprises entre 0,05 et 1,0 % (m/m) dans les aciers et les fontes solubles dans l'un ou l'autre des mélanges d'acide alternatifs.
Jeklo in lito železo - Določevanje celotnega silicija - Spektrofotometrična metoda (z reduciranim molibdo-silikatom) - 1. del: Deleži silicija 0,05 do 1 % (ISO 4829-1:1986)
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Standards Content (Sample)
SLOVENSKI STANDARD
01-december-1997
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Steel and cast iron - Determination of total silicon content - Reduced molybdosilicate
spectrophotometric method - Part 1: Silicon content between 0,05 and 1% (ISO 4829-
1:1986)
Eisen und Stahl - Ermittlung des Gesamtsiliziumgehaltes - Spektrophotometrisches
Verfahren (Reduzierte Molybdosilicate) - Teil 1: Siliziumgehalte zwischen 0,05 und 1%
(ISO 4829-1:1986)
Aciers et fontes - Détermination de la teneur en silicium total - Méthode
spectrophotométrique par molybdosilicate réduit - Partie 1: Teneur en silicum entre 0,05
et 1% (ISO 4829-1:1986)
Ta slovenski standard je istoveten z: EN 24829-1:1990
ICS:
77.040.30 Kemijska analiza kovin Chemical analysis of metals
77.080.01 Železne kovine na splošno Ferrous metals in general
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
International Standard 4829/ 1
INTERNATIONAL ORGANIZATION FOR STANDARDIZATIONWvlEIK~YHAPO~HAR OPrAHbl3AL&lR I-IO CTAHfiAPTM3AUWl.ORGANISATION INTERNATIONALE DE NORMALISATION
Steel and cast iron - Determination of total Silicon
- Reduced molybdosilicate spectrophotometric
content
method -
Part 1 : Silicon contents between 0,05 and 1,0 %
- Dosage du silicium total - IWthode spectrophotom&rique au molybdosilicate reduit - Partie I : Teneurs en
Aciers et fontes
silicium entre Cl,05 et 1 ,O %
First edition - 1986-12-VII
UDC 669.1 : 669.782 : 543.42 Ref. No. ISO 4829/1-1986 (E)
Descriptors : steels, cast iron, Chemical analysis, determination of content, Silicon, spectrophotometric analysis.
Price based on 7 pages
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of
national Standards bodies (ISO member bedies). 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.
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 4829/1 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.
0 International Organkation for Standardkation, 1986 l
Printed in Switzerland
ISO 4829/1-1986 (EI
INTERNATIONAL STANDARD
Determination of total Silicon
and cast iron -
Reduced molybdosilicate spectrophotometric
Part “1 : Silicon contents between Op05 and 1,O %
Scope and field of application 4.2 Sodium Peroxide, particle size -500 Pm.
This International Standard specifies a spectrophotometric
4.3 Nitrit acid.
method using reduced molybdosilicate for the determination of
total Silicon in steel and cast iron.
Slowly add 150 ml of nitric acid, Q approximately I,40 g/mI, to
600 ml of water. Cool, dilute to 1 000 ml and mix.
The method is applicable to Silicon contents between 0,05 and
1,0 % (mlm) in steel and cast iron soluble in one or the other
4.4 Sulfuric acid.
of the alternative acid mixtures.
To 600 ml of water add cautiously, with stirring, 250 mI of
sulfuric acid, Q approximately IJ4 g/ml. Cool, dilute to
2 Reference
1 000 ml and mix.
ISO 377, Wrought steel - Selection and preparation of
4.5 Sulfuric acid.
samples and test pieces.
To $06 ml of water add cautiously, with stirring, 50 ml of
sulfuric acid, e approximately 1,84 g/ml. Cool, dilute to
3 Principle
1 066 ml and mix.
Dissolution of a test Portion in an acid mixture appropriate to
4.6 Hydrochlorit acidhitric acid rnixture.
the alloy composition.
Fusion of the acid-insoluble residue with sodium Peroxide. Add 180 ml of hydrochloric acid, Q about IJ9 g/ml, and 65 ml
of nitric acid, Q about I,40 g/ml, to 500 ml of water, cool,
Formation of the oxidized molybdosilicate (yellow) in weak acid dilute to 1 000 ml and mix.
solution.
4.7 Sulfuric acidhitric acid mixture.
Selective reduction of the molybdosilicate complex to reduced
blue complex with ascorbic acid, after increasing the sulfuric
To 500 ml sf water add cautiously, with stirring, 35 rd of
acid concentration and adding oxalic acid to prevent the
sulfuric acid, Q about 1,84 g/ml, and 45 ml sf nitric acid,
interference of phosphorus, arsenic and vanadium.
Q about 1,4O g/ml. Cool, dilute to 1 CKN ml and mix.
Spectrophotometric measurement of the reduced blue complex
Ascorbic acid, 20 g/l Solution.
4.8
at a wavelength of about 810 nm.
ßrepare this Solution immediately before use.
4 Reagents
4.9 Bxallic acid solution.
During the analysis, unless otherwise stated, use only reagents
Dissolve 5 g of oxalic acid dihydrate K+-1204~21-120) in water,
of recognized analytical grade and only distilled water or water
dilute to 100 ml and mix.
of equivalent purity.
All solutions shall be freshly prepared and stored in
4.40 Hydrogen Peroxide.
polypropylene or polytetrafluoroethylene Containers.
Dilute 200 ml of hydrogen Peroxide, 300 g/l, to 1 000 ml and
4.1 Pure iron, Silicon content Iess than 5 pg/g. mix.
ISO 4829/1-1986 (EI
Spectrophotometer
4.11 Potassium permanganate, 22,5 g/l solution. 5.3
Filter before use. 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 ac-
4.12 Sodium molybdate Solution.
curate to +2 nm as measured by the absorption maximum of a
didymium filter at 803 nm, or other suitable calibration method.
Dissolve 2,5 g of sodium molybdate dihydrate
The absorption measurement for the Solution of maximum ab-
(Na2Mo04m2H20) in 50 ml sf water and filter through a
sorbance shall have a repeatability expressed as relative devi-
medium-texture filter Paper. Immediately before use, add 15 ml
ation of +0,3 % or bettet-.
of the sulfuric acid (4.5), dilute to 100 ml and mix.
4.13 Silicon, Standard Solution.
6 Sampling
Carry out sampling in accordan ce with ISO 377 or appropriate
4.13.1 Silicon, stock Solution corresponding to 1 g of Si per
national Standards for cast iron
litre.
Weigh, to the nearest 0,l mg, 2,139 3 g of freshly calcined
high-purity silica ( > 99,9 % SiO$ (see note 1) and transfer to a
7 Procedure
platinum crucible. Mix thoroughly with 16 g of anhydrous
sodium carbonate and fuse at 1 050 OC for 30 min. Extract the
7.1 Test portion
fusion product with 100 ml of water in a polypropylene or
polytetrafluoroethylene beaker (sec note 2). Transfer the ex-
Weigh, to the nearest 0,001 g, 0,50 + 0,Ol g (m) of test
tract, which should contain no trace of residue, to a 1 000 ml
Sample in the form of fine Chips, turnings, millings or filings.
one-mark volumetric flask, dilute to the mark and mix. Transfer
immediately to a weil-stoppered polytetrafluoroethylene bottle
for storage.
7.2 Blank test
1 ml of this stock Solution contains 1 mg of Si.
In parallel with the determination and following the same pro-
cedure, carry out a blank test using the same quantities of all
the reagents but using 0,50 + 0,Ol g of the pure iron (4.1) (see
4.13.2 Silicon, Standard solution corresponding to 200 mg of
note) instead of the test Portion.
Si per litre.
NOTE - Pure iron dissolves very slowly in the sulfuric acid/nitric acid
Transfer 50 ml of the Silicon stock Solution (4.13.1) to a 250 ml
mixture (4.7). lt may be dissolved in 85 ml of the sulfuric acid (4.5)
one-mark volumetric flask. Dilute to the mark and mix. Transfer
followed by 35 ml of the nitric acid (4.3).
immediately to a weil-stoppered polytetrafluoroethylene bottle
for storage.
7.3 Determination
1 ml of this Standard Solution contains 200 Mg of Si.
7.3.1 Dissolution of the test Portion
NOTES
Transfer the test Portion (7.1) into a 250 ml polypropylene or
1 The high-purity silica shall be
calcined for 1 h at 1 100 “C and
polytetrafluoroethylene beaker (5.1), add 120 ml sf the sulfuric
cooled in a desiccator immediately before use.
acid/nitric acid mixture (4.7) and warm gently to dissolve the
2 Extraction of the fusion product require prolonged digestion in
maY
test Portion (see notes 1 and 2).
wa ter followed by gentle heating.
When solvent action ceases, filter the Solution through a
hardened close-texture filter Paper of known low ash content
and collect the filtrate in a 500 ml beaker. Rinse the beaker with
5 Apparatus
20 ml of hot water, remove adherent particles with a rubber-
tipped rod, and filter the rinsings through the same filter Paper.
Ordinary laboratory apparatus and
Wash the filter Paper several times with 20 ml quantities of hot
water. Keep the filtrate for use in the procedure given in 7.3.3
(sec note 3).
5.1 Beakers, of polypropylene or polytetrafluoroethylene, of
250 ml capacity.
NOTES
1 For test portions slow to dissolve, the test Portion may be dissolved
in 85 ml of the sulfuric acid (4.5) followed by 35 ml of the nitric acid
5.2 Crucibles, of zirconium metal (see note), of 50 ml
(4.3).
capacity.
2 For test portions not soluble in the sulfuric acid/nitric acid mixture
NOTE - Sintered alumina crucibles may be used as alternatives to zir- (4.7), use instead 85 ml of the hydrochloric acid/nitric acid mixture
conium metal crucibles. (4.6).
ISO 4829/1-1986 (EI
3 If acid-soluble Silicon only is required, proceed directly to 7.3.3, but Dilute to the mark and mix. Allow each test Solution (test por-
the method for acid-soluble Silicon is unsatisfactory as different values tion and blank) and respective compensating Solution to stand
could be obtain
...
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