EN ISO 10280:1995
(Main)Steel and iron - Determination of titanium content - Diantipyrylmethane spectrophotometric method (ISO 10280:1991)
Steel and iron - Determination of titanium content - Diantipyrylmethane spectrophotometric method (ISO 10280:1991)
Migrated from Progress Sheet (TC Comment) (2000-07-10): Will be submitted to the UAP procedure to replace EU 182
Stahl und Eisen - Bestimmung von Titan - Photometrische Methode mit Diantipyrylmethan (ISO 10280:1991)
Diese internationale Norm beschreibt ein Verfahren zur Bestimmung von Titan in Stahl und Eisen mit Hilfe der Spektralphotometrie unter Verwendung von Diantipyrylmethan. Das Vefahren ist für Titangehalte zwischen 0,002 und 0,8% (Masenprozent) anwendbar.
Aciers et fontes - Dosage du titane - Méthode spectrophotométrique au diantipyrylméthane (ISO 10280:1991)
La présente Norme internationale prescrit une méthode spectrophotométrique de dosage du titane au diantipyrylméthane dans les aciers et les fontes. La méthode est applicable aux teneurs en titane comprises entre 0,002 % (m/m) et 0,80 % (m/m).
Jeklo in železo - Določanje titana - Spektrofotometrijska metoda z diantipirilmetanom (ISO 10280:1991)
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 10280:1998
01-avgust-1998
-HNORLQåHOH]R'RORþDQMHWLWDQD6SHNWURIRWRPHWULMVNDPHWRGD]
GLDQWLSLULOPHWDQRP ,62
Steel and iron - Determination of titanium content - Diantipyrylmethane
spectrophotometric method (ISO 10280:1991)
Stahl und Eisen - Bestimmung von Titan - Photometrische Methode mit
Diantipyrylmethan (ISO 10280:1991)
Aciers et fontes - Dosage du titane - Méthode spectrophotométrique au
diantipyrylméthane (ISO 10280:1991)
Ta slovenski standard je istoveten z: EN ISO 10280:1995
ICS:
77.080.01 Železne kovine na splošno Ferrous metals in general
SIST EN ISO 10280:1998 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 10280:1998
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SIST EN ISO 10280:1998
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SIST EN ISO 10280:1998
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SIST EN ISO 10280:1998
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SIST EN ISO 10280:1998
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SIST EN ISO 10280:1998
INTERNATIONAL
10280
STANDARD
First edition
1991-05-01
Steel and iron - Determination of titanium
content - Diantipyrylmethane
spectrophotometric method
- MHhode specfropl7otom~frique
Aciers et fontes - Dosage du Mane
au diantipyryim6thane
--_____._ -- -.--.
---.-Y-P------.
-____-
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~-
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Reference number
--
IS0 10280:1991(E)
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SIST EN ISO 10280:1998
IS0 10280:1991(E)
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. IS0 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 voting. Publication as an lnter-
national Standard requires approval by at least 75 % of the member
bodies casting a vote.
International Standard IS0 10280 was prepared by Technical Committee
ISO/TC 17, steel.
Annexes A and B of this International Standard are for information only.
0 is0 1991
All rights reserved. No part of this publication may be reproduced or utilized in any form
or by any means, electronic or mechanical, including photocopying and microfilm, without
permission in writing from the publisher.
International Organization for Standardization
Case Postale 56 l CH-1211 Genhe 20 l Switzerland
Printed in Switzerland
ii
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SIST EN ISO 10280:1998
IS0 10280:1991 (E)
INTERNATIONAL STANDARD
Steel and iron - Determination of titanium content -
Diantipyrylmethane spectrophotometric method
1 Scope 3 Principle
This International Standard specifies a diantipyryl- Dissolution of a test portion in hydrochloric, nitric
methane spectrophotometric method for the deter- and sulfuric acids.
mination of titanium in steel and iron.
Fusion of the residue with potassium hydrogen sul-
fate.
The method is applicable to titanium contents be-
tween 0,002 % (m]m) and 0,80 % (m/m).
Formation of a yellow complex with 4,4’-
diantipyrylmethane.
Spectrophotometric measurement of the coloured
complex at a wavelength of about 385 nm.
2 Normative references
4 Reagents
The following standards contain provisions which,
During the analysis, unless otherwise stated, use
through reference in this text, constitute provisions
only reagents of recognized analytical grade and
of this International Standard. At the time of publi-
only grade 2 water as specified in IS0 3696.
cation, the editions indicated were valid. All stan-
dards are subject to revision, and parties to
agreements based on this International Standard 4.1 Iron, of high purity containing less than
are encouraged to investigate the possibility of ap- 2 pg Ti/g.
plying the most recent editions of the standards in-
dicated below. Members of IEC and IS0 maintain
4.2 Potassium hydrogen sulfate (KHSO,).
registers of currently valid International Standards.
4.3 Sodium carbonate (Na,CO,), anhydrous.
IS0 377-2:1989, Selection and preparation of samples
and test pieces of wrought steels - Part 2: Samples
for the determination of the chemical composition.
4.4 Hydrochloric acid, p about 1 ,I 9 g/ml.
IS0 385~1:1984, Laboratory glassware - Ebreftes -
4.5 Nitric acid, p about I,40 g/ml.
Part 1: General requirements.
4.6 Hydrofluoric acid, p a bout 1 ,I 5 g/ml.
IS0 648: 1977, Laboratory glassware - One-mark
pipettes.
4.7 Hydrochloric acid, p about I,19 g/ml, diluted
IS0 1042: 1983, Laboratory glassware - One-mark 1 -t- I.
volumetric flasks.
4.8 Hydrochloric acid, p about I,19 g/ml, diluted
IS0 3696:1987, Water for analytical laboratory use -
1 + 3.
Specification and test methods.
4.9 Sulfuric acid, p about I,84 g/ml, diluted 1 + 1.
IS0 5725:1986, Precision of test methods - Determi-
nation of repeatability and reproducibility for a stan-
dard test method by inter-laboratory tests. 4.10 Tartaric acid solution, 100 g/l.
1
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SIST EN ISO 10280:1998
IS0 10280:1991(E)
4.11 Ascorbic acid solution, 100 g/l.
5 Apparatus
Prepare this solution immediately before use.
All volumetric glassware shall be class A, in ac-
cordance with IS0 385-1, IS0 648 or IS0 1042 as
appropriate.
4.12 Ammonium oxalate solution.
Ordinary laboratory apparatus, and
Dissolve 6 g of ammonium oxalate monohydrate
[(COONH&.H,O] in water and dilute to 200 ml.
5.1 Crucible, of platinum metal or platinum-gold
alloy, of capacity 30 ml.
4.13 Iron solution, 12,5 g/l.
5.2 Spectrophotometer.
Dissolve I,25 g of iron (4.1) in 10 ml of hydrochloric
acid (4.7) while heating gently. Add 5 ml of nitric acid
The spectrophotometer shall be equipped to meas-
(4.5) and boil until the volume of the solution is ap-
ure absorbance at a wavelength of 385 nm.
proximately 10 ml. Cool, transfer to a 100 ml one-
Wavelength measurement shall be accurate to
mark volumetric flask, dilute to the mark with water
+ 2 nm or less. In the absorbance range O,O5 to 0,85,
and mix.
absorbance measurements shall be repeatable to
+ 0,003 or better.
-
4.14 Reagent blank solution.
6 Sampling
Prepare a reagent blank solution in parallel with the
determination, using the same quantities of re-
Carry out sampling in accordance with IS0 377-2 or
agents as those used for the determination but no
appropriate national standards for steel and iron.
iron. Follow exactly the procedure described in 7.3.1
and 7.3.2, diluting to 100 ml with water.
7 Procedure
4.15 Diantipyrylmethane solution.
7.1 Test portion
Dissolve 4 g of 4,4’-methylenebis(2,3-dimethyl-l-
Weigh, to the nearest 0,0005 g, a test portion ac-
phenyl-5-pyrazolone) monohydrate, C,,H,,O,N,.H,O,
cording to the presumed titanium content as follows:
(diantipyrylmethane) in 20 ml of hydrochloric acid
(4.7) and dilute to 100 ml with water.
a) for titanium contents in the range 0,002 % (FTI/FTI)
to 0,125 % (FTI/FTZ), a test portion of 1 ,OO g;
4.16 Titanium standard solution
b) for titanium contents in the range 0,125 % (m/m)
to 0,80 % (IT-?/~?), a test portion of 0,50 g.
4.16.1 Titanium stock solution, corresponding to
1 g of Ti per Iitre.
7.2 Blank test
Weigh, to the nearest 0,000 1 g, 0,500 g of high purity
In parallel with the determination and following the
titanium metal [purity > 99,9 % (m/m)] and transfer
same procedure, carry out a blank test using the
to a 300 ml beaker. Add 180 ml of sulfuric acid, p
same quantities of all the reagents and the same
about I,84 g/ml, diluted I + 3, cover with a
cell as in the determination, substituting an equiv-
watchglass, heat gently until the metal has dissolved
alent amount of iron (4.1) for the test portion.
and oxidize with nitric acid (4.5) added drop by drop.
Cool, transfer to a 500 ml one-mark volumetric flask,
73 . Determination
dilute to the mark with water and mix.
1 ml of this stock solution contains I,0 mg of Ti.
7.3.1 Dissolution of the test portion
Place the test portion (7.1) in a 250 ml beaker. Add
4.16.2 Titanium standard solution, corresponding to
20 ml of hydrochloric acid (4.4), cover the beaker
50 mg of Ti per litre.
with a watchglass and digest at 70 OC to 90 OC until
the solvent action ceases. Add 5 ml of nitric acid
Transfer IO,0 ml of titanium stock solution (4.16.1) to
(4.5) and boil until the volume of the solution is ap-
a 200 ml one-mark volumetric flask. Dilute to the
proximately 10 ml.
mark with water and mix.
Cool the solution, add 20 ml of sulfuric acid (4.9) and
Prepare this solution immediately before use.
evaporate until fumes of sulfur trioxide appear. Just
before fuming occurs, solids will begin to form and
1 mI of this standard solution contains 50 pg of Ti.
2
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SIST EN ISO 10280:1998
IS0 10280:1991(E)
the following additions by means of burettes or
gentle heating is required to avoid spurting. Once
pipettes, swirling after each addition.
fuming begins the mixture becomes stable and may
be fumed briefly at a higher temperature. Avoid
a) Test solution:
overfuming, particularly with chromium-bearing al-
loys, as the chromium salts deposited are difficult to
-
iron solution (4.13) if required (see table 1);
redissolve.
Cool, add 20 ml of hydrochloric acid (4.8) and warm
- reagent blank solution (4.14) if required (see
to redissolve the salts.
table 1);
Filter through a low ash, medium texture filter paper
-- 2,0 ml of ammonium oxalate solution (4.12);
and wash with hot water. Wash with 10 ml of
hydrochloric acid (4.7) and again with hot water.
- 6,0 ml of hydrochloric acid (4.7);
Retain the filtrate.
- 8,0 ml of ascorbic acid solution (4.11), allow
7.3.2 Treatment of insoluble residue
to stand for 5 min;
Transfer the filter paper and residue to a crucible
- IO,0 ml of diantipyrylmethane solution (4.15).
(5.1), dry and ignite at as low a temperature as
possible until all carbonaceous matter is removed
b)
...
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