EN ISO 10700:1995
(Main)Steel and iron - Determination of manganese content - Flame atomic spectrometric method (ISO 10700:1994)
Steel and iron - Determination of manganese content - Flame atomic spectrometric method (ISO 10700:1994)
The principle of the method specified is dissolving a test portion in hydrochloric and nitric acids followed by evaporation with perchloric acid until white fumes appear, spraying the solution into an air-acetylene flame, spectrometrically measuring the atomic absorption of the 279,5 nm spectral line emitted by a manganese hollow cathode lamp. The method is applicable to manganese contents between 0,002 % (m/m) and 2,0 % (m/m).
Stahl und Eisen - Bestimmung von Mangan - Flammenatomabsorptionsspektrometrisches Verfahren (ISO 10700:1994)
Diese internationale Norm beschreibt ein Verfahren zur Bestimmung des Mangangehaltes in Stahl und Eisen mit Hilfe der Flammen-Atomabsorptions- spektrometrie. Das Verfahren ist anwendbar für Mangangehalte zwischen 0,002 und2%.
Aciers et fontes - Dosage du manganèse - Méthode par spectrométrie d'absorption atomique dans la flamme (ISO 10700:1994)
La présente Norme internationale prescrit une méthode par spectrométrie d'absorption atomique dans la flamme pour le dosage du manganèse dans les aciers et les fontes. La méthode est applicable aux teneurs en manganèse comprises entre 0,002 % (m/m) et 2,0 % (m/m).
Jeklo in železo - Določanje mangana - Metoda s plamensko atomsko spektrometrijo (ISO 10700:1994)
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
01-avgust-1998
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VSHNWURPHWULMR ,62
Steel and iron - Determination of manganese content - Flame atomic spectrometric
method (ISO 10700:1994)
Stahl und Eisen - Bestimmung von Mangan -
Flammenatomabsorptionsspektrometrisches Verfahren (ISO 10700:1994)
Aciers et fontes - Dosage du manganese - Méthode par spectrométrie d'absorption
atomique dans la flamme (ISO 10700:1994)
Ta slovenski standard je istoveten z: EN ISO 10700:1995
ICS:
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 ISO
STANDARD 10700
First edition
1994-05-15
- Determination of
Steel and iron
manganese content - Flame atomic
absorption spectrometric method
- Dosage du manganese - Mkthode par spectrom&rie
Aciers et fon tes
d ‘absorption atomique dans Ia flamme
Reference number
ISO 10700:1994(E)
ISO 10700:1994(E)
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, governmental
and non-governmental, in liaison with ISO, also take part in the work. ISO
collaborates closely with the International Electrotechnical Commission
fl EC) 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 International
Standard requires approval by at least 75 % of the member bodies casting
a vote.
International Standard ISO 10700 was prepared by Technical Committee
ISO/TC 17, Steel, Subcommittee SC 1, Methods of determination of
Chemical composition.
Annex A forms an integral part of this International Standard. Annexes B
and C are for information 0 nly.
0 ISO 1994
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced
or utilized in any form or by any means, electronie or mechanical, including photocopying and
microfilm, without Permission in writing from the publisher.
International Organization for Standardization
Case Postale 56 l CH-l 211 Geneve 20 l Switzerland
Printed in Switzerland
ii
INTERNATIONAL STANDARD 0 ISO ISO 10700:1994(E)
Steel and iron - Determination of manganese
content - Flame atomic absorption spectrometric
method
De ter-
ISO 5725:1986, Precision of test methods -
1 Scope
for a
mina tion of repea tability and reproducibility
Standard test method by inter-laboratory tests.
This International Standard specifies a flame atomic
absorption spectrometric method for the deter-
mination of the manganese content in steel and iron.
3 Principle
The method is applicable to manganese contents be-
Dissolution of a test Portion in hydrochloric ana nrrrtc
tween 0,002 % (m/m) and 2,0 % (m/m).
acids followed by evaporation with perchloric acid
until white fumes appear.
Spraying of the Solution into an air-acetylene flame.
2 Normative references
Spectrometric measurement of the atomic absorption
of the 279,5 nm spectral line emitted by a manganese
The following Standards contain provisions which,
hollow cathode lamp.
through reference in this text, constitute provisions
of this International Standard. At the time of publi-
cation, the editions indicated were valid. All Standards
4 Reagents
are subject to revision, and Parties to agreements
based on this International Standard are encouraged
During the analysis, unless otherwise stated, use only
to investigate the possibility of applying the most re-
reagents of recognized analytical grade and only grade
cent editions of the Standards indicated below.
2 water as specified in ISO 3696.
Members of IEC and ISO maintain registers of cur-
rently valid International Standards.
4.1 Pure iron, free from manganese or with a
known low manganese content.
ISO 377-2: 1989, Selection and preparation of samples
and test pieces of wrought steels - Part 2: Samples
for the determination of the Chemical composition.
4.2 Hydrochlorit acid, p about IJ 9 g/ml.
ISO 385-1: 1984, Laboratory glassware - Burettes -
4.3 Hydrofluoric acid, p about 1 ,I 5 g/ml.
Part 1: General requiremen ts.
ISO 648: 1977, Laboratory glassware - One-mark
4.4 Nitrit acid, p about 1,40 g/ml.
pipettes.
ISO 1042: 1983, Laboratory glassware - One-mark
4.5 Perchlorit acid, p about 1,54 g/ml (see note 1).
volumetric flasks.
NOTE 1
Perchlorit acid (p about 1,67 g/ml) may also be
ISO 3696: 1987, Water for analytical laboratory use - used. 100 ml of perchloric acid (p about 1,54 g/ml) is
equivalent to 79 ml of perchloric acid (p about 1,67 g/ml).
Specifica tion and test methods.
ISO 10700:1994(E)
4.6 Background Solution. Ordinary laboratory apparatus, and
WARNING - See clause 7.
5.1 Atomic absorption spectrometer, equipped
with a manganese hollow cathode lamp and supplied
Weigh, to the nearest 0,Ol g, 10,OO g of the pure iron
with air and acetylene sufficiently pure to give a
(4.1). Place in a 1 litre beaker. Add 200 ml of
steady clear fuel-lean flame, free from water and Oil,
hydrochloric acid (4.2), cover the beaker with a watch
and free from manganese.
glass and heat gently until the iron is dissolved. Then
oxidize by adding 50 ml of nitric acid (4.4) in small
The atomic absorption spectrometer used will be sat-
portions. Add 150 ml of perchloric acid (4.5). Heat
isfactory if, after optimization according to 7.3.5, the
strongly and evaporate until dense white fumes of
limit of detection and characteristic concentration are
perchloric acid appear. Continue fuming for 15 min at
in reasonable agreement with the values given by the
a temperature that maintains a steady reflux of white
manufacturer and it meets the precision criteria given
perchloric acid fumes on the Walls of the beaker. Al-
in 5.1.1 to 5.1.3.
low to cool, add 300 ml of water and heat gently to
dissolve the salts.
lt is also desirable that the instrument should conform
to the additional Performance requirements given in
Transfer quantitatively to a 1 000 ml one-mark
5.1.4.
volumetric flask. Dilute to the mark with water and
5.1.1 Minimum precision (see A.l)
ckgro und Solution contains 0,010 g of
1 ml of this ba
Calculate the Standard deviation of 10 measurements
Fe .
of the absorbance of the most concentrated cali-
bration Solution. The Standard deviation shall not ex-
4.7 Manganese, Standard Solution.
ceed 1,5 % of the mean absorbance of this Solution.
Calculate the Standard deviation of 10 measurements
4.7.1 Manganese stock Solution, corresponding to
of the absorbance of the least concentrated calibration
l,OO g of Mn per Iitre.
Solution (excluding the Zero member). The Standard
Weigh, to the nearest 0,l mg, 1 ,OO g of pure
deviation shall not exceed 0,5 % of the mean
manganese metal [purity 3 99,9 % (m/m)]. Place in a
absorbance of the most concentrated calibration sol-
250 ml beaker and add 40 ml of hydrochloric acid
ution.
(4.2). Cover with a watch glass and heat gently until
the manganese has dissolved. Cool, transfer the sol-
5.1.2 Limit of detection (see A.2)
ution quantitatively to a 1 000 ml one-mark volumetric
flask, dilute to the mark with water and mix.
This is defined as twice the Standard deviation of 10
measurements of the absorbance of a Solution con-
1 ml of this Standard Solution contains 1,00 mg of
taining the appropriate element at a concentration
Mn .
level selected to give an absorbance just above that
of the Zero member.
4.7.2 Manganese Standard Solution, correspond-
ing to 0,02 g of Mn per Iitre. The limit of detection of manganese in a matrix similar
to the final test Portion Solution shall be less than
Transfer 20,O ml of the stock Solution (4.7.1) to a
0,02 pg of Mn per millilitre.
1 000 ml one-mark volumetric flask, dilute to the mark
with water and mix.
5.1.3 Graph linearity (see A.3)
Prepare this Standard Solution immediately before
The value of the slope of the calibration graph cover-
use.
ing the top 20 % of the concentration range (ex-
pressed as a Change in absorbance) shall not be less
1 ml of this Standard Solution contains 0,02 mg of
than 0,7 times the value of the slope for the bottom
Mn .
20 % of the concentration range (expressed as a
Change in absorbance) determined in the same way.
5 Apparatus
For instruments with automatic calibration using two
All volumetric glassware shall be class A, in accord- or more Standards, it shall be established Prior to the
analysis, by obtaining absorbance readings, that the
ante with ISO 385-1, ISO 648 or ISO 1042, as appro-
above requirements for graph linearity are fulfilled.
priate.
0 ISO
ISO 10700:1994(E)
5.1.4 Characteristic concentration (see A.4) a watch glass and heat gently until solvent action
ceases. Add 5 ml of nitric acid (4.4), and boil for
The characteristic concentration of manganese in a
1 min to remove oxides of nitrogen. Add 15 ml of
matrix similar to the final test Portion Solution shall be
perchloric acid (4.5), and heat strongly without a cover
better than 0,l pg of Mn per millilitre.
until fuming commences. Cover with a watch glass
and continue heating at a temperature at which a
5.2 Ancillary equipment steady reflux of white perchloric acid fumes is main-
tained on the Walls of the beaker. Continue heating
A Strip Chart recorder and/or digital readout device is
until there are no perchloric acid fumes visible inside
recommended to evaluate the criteria in 5.1 .l to 5.1.3
the beaker.
and for all subsequent measurements.
For samples not readily soluble in hydrochloric acid
Scale expansion tan be used until the noise observed
and nitric acid, add 2 ml of hydrofluoric acid (4.3) be-
is greater than the read-out error and is always rec-
fore the addition of 15 ml of perchloric acid and con-
ommended for absorbances below 0,l. If scale ex-
tinue as described above.
pansion has to be used and the instrument does not
have the means to read the value of the scale expan-
7.3.2 Treatment of the Solution
sion factor, the value tan be calculated by measuring
the absorbances of a suitable Solution with and with-
7.3.2.1 Manganese contents up to 0,lO % (m/m)
out scale expansion and using the ratio of the Signals
obtained.
Allow to cool, add 25 ml of water and heat gently to
dissolve the salts. Cool again and transfer
6 Sampling
quantitatively to a 250 ml one-mark volumetric flask.
Dilute to the mark with water and mix.
in accordance with ISO 377-2 or
Carry out sampling
Standards for steel and iron.
appropriate national
Filter by decantation through a dry, medium-texture
filter Paper to remove any residue or precipitate, and
collect the filtrate in a dry beaker after discarding the
7 Procedure
first portions.
WARNING - Perchlorit acid vapour may Cause
The filtrate is the test Solution for determining
explosions in the presence of ammonia, nitrous
manganese contents up to 0,lO % (4~2).
fumes or organic matter in general. All evap-
orations must be carried out in fume cupboards
7.3.2.2 Manganese contents between
suitable for use with perchloric acid.
0,lO % (m/m) and 0,40 % (m/m)
Ensure that the Spray System and drainage System
Transfer 50,O ml of the filtrate (7.3.2.1) to a 200 ml
are washed free from perchloric acid after use.
one-mark volumetric flask, dilute to the mark with
water and mix.
7.1 Test Portion
7.3.2.3 Manganese contents between
imately 1,0 g of
Weigh, to the nearest 1 mg, a
PProx
0,40 % (m/m) and 2,0 % (m/m)
the test sa mple.
Transfer IO,0 ml of the filtrate (7.3.2.1) to a 200 ml
7.2 Blank test
one-mark volumetric flask, dilute to the mark with
water and mix.
In parallel with the determination and following the
Same procedure, carry out a blank test using the same
7.3.3 Preparation of the calibration solutions
quantities of all the reagents, including the pure iron
(4.1).
7.3.3.1 Manganese contents up to 0,lO % (m/m)
7.3 Determination
Introduce 40,O ml of the background Solution (4.6)
into a series of eight 100 ml one-mark volumetric
7.3.1 Preparation of the test Solution
flasks. Using a burette or pipette, add the volumes of
manganese Standard Solution (4.7.2) indicated in
Place the test Portion (7.1) in a 250 ml beaker. Add
table 1. Dilute to the mark with water and mix.
20 ml of hydrochloric acid (4.2), cover the beaker with
ISO 10700:1994(E)
Table 1 Table 3
Volume of
Corresponding
manganese
Mass of content of
Standard
manganese manganese in
manganese
solution
test Sample
(4.7.2)
ml % (dm)
0') 0 0
0,40
410 0,08
8,O 0,16 0,80
12,o 1,20
0,24
16,O 0,32 1,60
20,o 0,40 2,00
1) Zero member.
1) Zero member.
7.3.4 Adjustment of atomic absorption
spectrometer
7.3.3.2 Manganese contents between
See table4.
0,lO % (m/m) and 0,40 % (m/m)
Introduce IO,0 ml of the background Solution (4.6)
Table 4
into a series of six 100 ml one-mark volumetric flasks.
Using a burette or pipette, add the volumes of
Element Characteristic
manganese Standard Solution (4.7.2) indicated in
Type of lamp Manganese hollow cathode
table2. Dilute to the mark with water and mix.
Wayelength 279,5 nm
Air-acetylene fuei-lean flame ad-
Flame
Table 2
justed for maximum manganese
response
Lamp current Follow manufacturer ’s recommen-
dations
manganese
Bandwidth Follow manufacturer ’s recommen-
dations
ml % (dm)
0') 0 0
manufacturer ’s recommendations
0,08 0,08
fol!owed and particular attention
0,16 O,l6
is drawn to the following safety Points:
12,o 0,24 0,24
a) the explosive nature sf acetylene, and regu-
16,O 0,32 0,32
la
...
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