EN 24943:1990
(Main)Chemical analysis of ferrous metal - Determination of copper content - Flame atomic absorption spectrometric method (ISO 4943:1985)
Chemical analysis of ferrous metal - Determination of copper content - Flame atomic absorption spectrometric method (ISO 4943:1985)
The method is applicable to copper contents between 0.004 % (m/m) and 0.5 % (m/m). 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 includes the graphical representation of precision data.
Chemische Analyse des Eisen- und Stahlwerkstoffes - Ermittlung des Kupfergehalts - Flammenatomabsorptionsspektrometrisches Verfahren (ISO 4943:1985)
Verstaendigung und Kommunikation. Qualitaet.
Analyse chimique des matériaux sidérurgiques - Détermination de la teneur en cuivre - Méthode par spectrométrie d'absorption atomique dans la flamme (ISO 4943:1985)
La présente Norme internationale spécifie une méthode de dosage par spectrométrie d'absorption atomique dans la flamme, du cuivre dans les aciers et fontes. La méthode est applicable aux teneurs en cuivre comprises entre 0,004 et 0,5 % (m/m).
Kemična analiza železovih zlitin - Določevanje bakra - Plamenska atomska absorpcijska spektrometrična metoda (ISO 4943:1985)
General Information
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Standards Content (Sample)
SLOVENSKI STANDARD
01-december-1997
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Chemical analysis of ferrous metal - Determination of copper content - Flame atomic
absorption spectrometric method (ISO 4943:1985)
Chemische Analyse des Eisen- und Stahlwerkstoffes - Ermittlung des Kupfergehalts -
Flammenatomabsorptionsspektrometrisches Verfahren (ISO 4943:1985)
Analyse chimique des matériaux sidérurgiques - Détermination de la teneur en cuivre -
Méthode par spectrométrie d'absorption atomique dans la flamme (ISO 4943:1985)
Ta slovenski standard je istoveten z: EN 24943:1990
ICS:
77.040.30 Kemijska analiza kovin Chemical analysis of metals
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
International Standard
INTERNATIONAL ORGANIZATION FOR STANDARDIZATION.ME)I(JJYHAPOfiHAR OPrAHl’l3AlJMfl fl0 CTAHAAPTM3AUMM.ORGANlSATION INTERNATIONALE DE NORMALISATION
- Determination of topper content -
Steel and cast iron
Flame atomic absorption spectrometric method
- Dosage du cuivre - M&hode par spectrom&rie d’absorption atomique dans Ia flamme
Aciers et fon tes
First edition - 1985-12-15
Ref. No. ISO 4943-1985 (E)
UDC 669.13/14: 543.422 : 546.56
Descriptors : steels, cast iron, Chemical analysis, determination of content, topper, atomic absorption method.
Price based on 6 pages
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 patt 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 4943 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, 1985 l
Printed in Switzerland
ISO 49434985 (E)
INTERNATIONAL STANDARD
- Determination of topper content -
Steel and cast iron
Flame atomic absorption spectrometric method
4.3 Hydrochlorit acid-nitric acid-perchloric acid
Scope and field of application
mixture.
This International Standard specifies a method for the deter-
Mix 20 ml of hydrochloric acid (Q about 1,19 g/ml) with 55 ml
mination of topper in steel and cast iron by means of flame
of nitric acid (Q about 140 g/ml) and 75 ml of perchloric acid
atomic absorption spectrometry.
(Q about 154 g/mlL
The method is applicable to topper contents in the range 0,004
NOTE - Perchlorit acid (Q about 1,67 g/ml) may also be used. 100 ml
to 0,5 % (mlm).
of perchloric acid (g about 1,54 g/ml) is equivalent to 79 ml of per-
chloric acid (Q about 1,67 g/ml).
2 Reference
4.4 Copper, Standard Solution.
ISO/R 377, Selection and preparation of samples and test
pieces for wrought steel.
4.4.1 Stock solution, corresponding to 1 g of Cu per litre.
Weigh, to the nearest 0,000 1 g, 1,000 0 g of high purity
3 Principle
topper [> 99,95 % Hrn) Cu].
Dissolution of a test Portion in a mixture of hydrochloric, nitric
Transfer to a 400 ml beaker and dissolve in 25 ml of nitric acid
and perchloric acids.
(Q about 140 g/ml, diluted 1 + 4). Cover with a watch-glass.
When dissolution is complete, evaporate on a water-bath until
Spraying of the Solution into an air-acetylene flame. Spec-
the onset of crystallization. Dissolve the residue in water, cool,
trometric measurement of the atomic absorption of the
transfer to a 1 000 ml one-mark volumetric flask, dilute to the
324,7 nm spectral Iine emitted by a topper hollow cathode
mark and mix.
lamp.
4.4.2 Standard Solution, corresponding to 20 mg of Cu per
litre.
4 Reagents
Transfer 20,O ml of the stock Solution (4.4.1) into a 1 000 ml
During the analysis, unless otherwise stated, use only reagents
one-mark volumetric flask, dilute to the mark and mix.
of recognized analytical grade and having a very low topper
content, and only distilled water or water of equivalent purity.
1 ml of this Standard Solution contains 20 pg of Cu.
If possible, use only freshly prepared distilled or de-ionized
Prepare this Standard Solution immediately before use.
water.
4.1 Iron of high purity,
topper content < 0,000 5 % (mlm).
5 Apparatus
Ordinary laboratory apparatus, and
4.2 Hydrochlorit acid-nitric acid mixture.
5.1 Atomic absorption spectrometer.
Mix three Parts by volume of hydrochloric acid (Q about
1,19 g/ml), one patt by volume of nitric acid (Q about
140 g/ml), and two Parts by volume of water. A topper hollow cathode lamp; supplies of air and acetylene
sufficiently pure to give a steady clear fuel-lean flame, free from
Prepare this mixture immediately before use. water and Oil, and free from topper.
ISO 4943-1985 (EI
The atomic absorption spectrometer used will be satisfactory if expansion factor, the value tan be calculated by measuring a
after optimization according to 7.3.4 the limit of detection and suitable Solution with and without scale expansion and simply
characteristic concentration are in reasonable agreement with dividing the Signal obtained.
the values given by the manufacturer and it meets the precision
criteria given in 5.1 .l.
6 Sampling
5.1.1 Minimum precision
Carry out sampling in accordance with ISO/R 377 or ap-
Calculate the Standard deviation of 10 measurements of the ab-
propriate national Standards for cast iron.
sorbance of the most concentrated calibration solution. The
Standard deviation shall not exceed 1,0 % of the mean ab-
sorbance.
7 Procedure
Calculate the Standard deviation of 10 measurements of the ab-
WARNING - Perchlorit acid vapour may Cause ex-
sorbance of the least concentrated calibration Solution
plosions in the presence of ammonia, nitrous fumes or
(excluding the zero member). The Standard deviation shall not
organic matter in general.
exceed 0,5 % of the mean absorbance of the most concen-
trated calibration solution.
Ensure that the Spray System and dra inage System are washed
free from perch loric acid after use.
lt is also
desirable that the instrument should conform to
the
additiona I Performance requirements.
given in 5.1.1.1 to
NOTE - All glassware shall first be washed in hydrochloric acid
5.1.1.3.
(Q about 1,19 g/ml, diluted 1 + 11, then in water. The quantity of cop-
per present in the beakers and flasks tan be checked by measuring the
5.1 .l .l Characteristic concentration
absorption of the distilled water introduced into the glassware after the
acid wash.
The characteristic concentration for topper in a matrix similar
to the final test Portion solution shall be better than 0,lO pg of
7.1 Test Portion
Cu per millilitre.
Weigh, to the nearest 0,001 g, approximately
0,5 g of the test
5.1.1.2 Limit of detection
Sample.
This is defined as twice the Standard deviation of
10 measurements of the absorbance of a Solution containing
7.2 Blank test
the appropriate element of a concentration level selected to
give an absorbance just above that of the zero member.
Parallel with the determination and following the same
procedure, carry out a blank test using the same quantities of
The limit of detection of topper in a matrix similar to the final
all the reagents.
test Portion Solution shall be better than 0,15 pg of Cu per
millilitre.
7.3 Determination
5.1 .1.3 Graph linearity
7.3.1 Preparation of the test Solution
The slope of the calibration graph covering the top 20 % of the
Place the test Portion (7.1) in a 250 ml beaker. Add, in small
concentration range (expressed as a Change in absorbance)
portions, 20 ml of the hydrochloric acid-nitric acid-perchloric
shall not be less than 0,7 times the value of the slope for the
acid mixture (4.3), cover the beaker with a watch-glass and
bottom 20 % of the concentration range (expressed as a
heat gently until solvent action ceases. Evaporate until dense
Change in absorbance) determined in the same way.
white fumes of perchloric acid appear. Continue fuming for
1 min at such a temperature as to maintain a steady reflux of
For instruments with automatic calibration using two or more
white perchloric acid fumes on the Walls of the beaker.
Standards, it shall be established Prior to the analysis, by ob-
taining absorbance readings, that the above requirements for
NOTE - For samples not readily soluble in the hydrochloric acid-nitric
graph linearity are fulfilled.
acid-perchloric acid mixture (4.31, first dissolve in 10 ml of the
hydrochloric acid-nitric acid mixture (4.2) before adding the 20 ml of
the hydrochloric acid-nitric acid-perchloric acid mixture (4.3).
52 .
Ancillary equipment.
A Strip Chart recorder and/or digital readout device is recom- Allow to cool, add 25 ml of water and heat gently to dissolve
salts. Cool again and transfer quantitatively to a 100 ml one-
mended to evaluate the criteria in 5.1.1 and for all subsequent
mark volumetric flask. Dilute to the mark and mix.
measurements.
Filter by decantation through a dry medium filter Paper to
Scale expansion tan be used until the noise observed is greater
remove any residue or pr
...
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