SIST EN 14242:2023
(Main)Aluminium and aluminium alloys - Chemical analysis - Inductively coupled plasma optical emission spectrometric analysis
Aluminium and aluminium alloys - Chemical analysis - Inductively coupled plasma optical emission spectrometric analysis
This European Standard describes detailed steps for dissolution and preparation of calibration solutions. The pre-ferred use is for certification and referee analysis. All instrumentation, including software used in the testing labo-ratories, are different an subject to change. Therefore, general criteria for calibration and measurement are speci-fied.
This method has to be used with primary reference materials whose mass of substance have a significant smaller uncertainty as required of the repeatability of the testing procedure.
Aluminium und Aluminiumlegierungen - Chemische Analyse - Optische Emissionsspektrometrie mit induktiv gekoppeltem Plasma
Dieses Dokument legt ein Verfahren für die optische Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-OES, en: inductively coupled plasma optical emission spectrometric method) zur Analyse von Aluminium und Aluminiumlegierungen fest.
Dieses Verfahren ist für die Bestimmung von Silicium, Eisen, Kupfer, Mangan, Magnesium, Chrom, Nickel, Zink, Titan, Gallium, Vanadium, Beryllium, Bismut, Calcium, Cadmium, Cobalt, Lithium, Natrium, Blei, Antimon, Zinn, Strontium und Zirconium in Aluminium und Aluminiumlegierungen anwendbar.
Der Gehalt der zu bestimmenden Elemente sollte mindestens 10-mal höher sein als die Nachweisgrenze des Verfahrens.
Aluminium et alliages d’aluminium - Analyse chimique - Analyse par spectrométrie d’émission optique avec source à plasma induit par haute fréquence
Le présent document spécifie une méthode par spectrométrie d’émission optique avec source à plasma
induit par haute fréquence (ICP-OES) pour l’analyse de l’aluminium et des alliages d’aluminium.
Cette méthode est applicable à la détermination de la teneur en silicium, fer, cuivre, manganèse,
magnésium, chrome, nickel, zinc, titane, gallium, vanadium, béryllium, bismuth, calcium, cadmium, cobalt,
lithium, sodium, plomb, antimoine, étain, strontium et zirconium dans l’aluminium et les alliages
d’aluminium.
Il convient que la teneur des éléments à déterminer soit au moins 10 fois supérieure aux limites de
détection de la méthode.
Aluminij in aluminijeve zlitine - Kemična analiza - Analiza s spektrometrijo optične emisije z induktivno sklopljeno plazmo
Ta evropski standard podrobno opisuje korake za raztapljanje in pripravo kalibracijskih raztopin. Prednostno se uporablja za certificiranje in analizo referenc. Vsi instrumenti, vključno s programsko opremo za preskuševalne laboratorije, se razlikujejo in so predmet sprememb. Za to so določena splošna merila za umerjanje in merjenje.
To metodo je treba uporabljati s prednostnimi referenčnimi materiali, katerih snovi ima bistveno manjšo stopnjo negotovosti, kot je potrebna za ponovljivost preskusnega postopka.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN 14242:2023
01-maj-2023
Aluminij in aluminijeve zlitine - Kemična analiza - Analiza s spektrometrijo optične
emisije z induktivno sklopljeno plazmo
Aluminium and aluminium alloys - Chemical analysis - Inductively coupled plasma optical
emission spectrometric analysis
Aluminium und Aluminiumlegierungen - Chemische Analyse - Optische
Emissionsspektrometrie mit induktiv gekoppeltem Plasma
Aluminium et alliages d’aluminium - Analyse chimique - Analyse par spectrométrie
d’émission optique avec source à plasma induit par haute fréquence
Ta slovenski standard je istoveten z: EN 14242:2023
ICS:
77.040.30 Kemijska analiza kovin Chemical analysis of metals
77.120.10 Aluminij in aluminijeve zlitine Aluminium and aluminium
alloys
SIST EN 14242:2023 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN 14242:2023
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SIST EN 14242:2023
EN 14242
EUROPEAN STANDARD
NORME EUROPÉENNE
March 2023
EUROPÄISCHE NORM
ICS 77.040.30; 77.120.10 Supersedes EN 14242:2004
English Version
Aluminium and aluminium alloys - Chemical analysis -
Inductively coupled plasma optical emission spectrometric
analysis
Aluminium et alliages d'aluminium - Analyse chimique Aluminium und Aluminiumlegierungen - Chemische
- Analyse par spectrométrie d'émission optique avec Analyse - Optische Emissionsspektrometrie mit
source à plasma induit par haute fréquence induktiv gekoppeltem Plasma
This European Standard was approved by CEN on 23 January 2023.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2023 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 14242:2023 E
worldwide for CEN national Members.
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SIST EN 14242:2023
EN 14242:2023 (E)
Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 4
5 Reagents . 5
6 Apparatus .10
7 Sampling .11
7.1 General .11
7.2 Test sample .11
8 Procedure.11
8.1 Test portion .11
8.2 Dissolution procedure I with sodium hydroxide solution .11
8.3 Dissolution procedure II with nitric acid and hydrofluoric acid .12
8.4 Dissolution procedure III with a mixture of hydrochloric acid and nitric acid .12
8.5 Dissolution procedure IV with hydrochloric acid .13
8.6 Calibration solutions and drift correction solution .13
8.6.1 General .13
8.6.2 Preparation of the calibration solutions .14
8.7 Measurements .14
8.7.1 Adjustment of the apparatus .14
8.7.2 Measurement of the calibration solutions .14
8.7.3 Measurement of the test solutions .15
8.8 Calibration curves .15
9 Correction of short-term fluctuations and drift .15
9.1 General .15
9.2 Short-term fluctuations .15
9.3 Drift .15
10 Investigation of interferences .15
11 Expression of the results .16
11.1 Correction .16
11.2 Result .16
12 Test report .16
Annex A (informative) Analytical wavelengths .17
Annex B (informative) Plasma optical emission spectrometer — Suggested performance
criteria to be checked .19
Bibliography .21
2
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SIST EN 14242:2023
EN 14242:2023 (E)
European foreword
This document (EN 14242:2023) has been prepared by Technical Committee CEN/TC 132 “Aluminium
and aluminium alloys”, the secretariat of which is held by AFNOR.
This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by September 2023, and conflicting national standards shall
be withdrawn at the latest by September 2023.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN 14242:2004.
The main changes compared to the previous edition are listed below:
— modification of the title and Scope;
— new subclause 5.15.6;
— several editorial modifications.
Any feedback and questions on this document should be directed to the users’ national standards body.
A complete listing of these bodies can be found on the CEN website.
According to the CEN-CENELEC Internal Regulations, the national standards organisations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia,
Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland,
Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of North
Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and the United
Kingdom.
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EN 14242:2023 (E)
1 Scope
This document specifies an inductively coupled plasma optical emission spectrometric method
(ICP-OES) for the analysis of aluminium and aluminium alloys.
This method is applicable to the determination of silicon, iron, copper, manganese, magnesium,
chromium, nickel, zinc, titanium, gallium, vanadium, beryllium, bismuth, calcium, cadmium, cobalt,
lithium, sodium, lead, antimony, tin, strontium and zirconium in aluminium and aluminium alloys.
The content of the elements to be determined should be at least 10 times higher than the corresponding
detection limits.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
EN 12258-2:2004, Aluminium and aluminium alloys - Terms and definitions - Part 2: Chemical analysis
EN 14361, Aluminium and aluminium alloys - Chemical analysis - Sampling from metal melts
EN ISO 648, Laboratory glassware - Single-volume pipettes (ISO 648)
EN ISO 1042, Laboratory glassware - One-mark volumetric flasks (ISO 1042)
EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696)
3 Terms and definitions
For the purposes of this document, the terms and definitions given in EN 12258-2:2004 apply.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— IEC Electropedia: available at https://www.electropedia.org/
— ISO Online browsing platform: available at https://www.iso.org/obp
4 Principle
A test portion is dissolved with:
— a sodium hydroxide solution followed by acidification with a mixture of nitric acid and hydrochloric
acid; or
— nitric acid and hydrofluoric acid; or
— a mixture of hydrochloric acid and nitric acid; or
— hydrochloric acid and hydrogen peroxide
according to the alloy type and the element to be determined.
After suitable dilution and, if necessary, addition of an internal reference element, the solution is
nebulized into an inductively coupled plasma optical emission spectrometer and the intensity of the
emitted light (including, where appropriate, that of the internal reference element) is measured. The
4
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EN 14242:2023 (E)
emission signals on the selected analytical lines (see Annex A) are then compared with those of the
calibration solutions.
NOTE 1 The ranges of application and the accuracy of the method or any alternative steps are validated by the
laboratory. Approximate ranges of application are given in Annex A.
NOTE 2 All instrumentation, including software used in the laboratories, are different and subject to change.
Therefore, only general criteria for calibration and measurement are specified.
5 Reagents
During the analysis, unless otherwise specified, use only reagents of recognized analytical grade and only
grade 2 water as specified in EN ISO 3696 or equivalent quality.
The same reagents should be used for preparation of calibration solutions and of sample solutions.
5.1 Aluminium, purity ≥ 99,999 % by mass.
5.2 Sodium carbonate (Na CO )
2 3
5.3 Potassium carbonate (K CO )
2 3
5.4 Sodium nitrite (NaNO )
2
5.5 Potassium disulphate (K S O )
2 2 7
5.6 Nitric acid, ρ = 1,40 g/ml approximately.
5.7 Nitric acid solution, 1 + 1
Carefully add 500 ml of nitric acid (5.6) to 400 ml water, allow to cool, dilute to 1 l with water and mix.
5.8 Nitric acid solution, 4 mol/l
Carefully add 27,7 ml of nitric acid (5.6) to 50 ml water, allow to cool, dilute to 100 ml with water and
mix.
5.9 Hydrochloric acid, ρ = 1,19 g/ml, approximately
5.10 Hydrochloric acid solution, 1 + 1
Carefully add 500 ml of hydrochloric acid (5.9) to 400 ml water, allow to cool, dilute to 1 l with water and
mix.
5.11 Hydrofluoric acid, ρ = 1,14 g/ml, approximately.
5.12 Sulphuric acid, ρ = 1,84 g/ml approximately.
5.13 Hydrogen peroxide, 30 % (by mass) solution.
5.14 Sodium hydroxide solution, 400 g/l
Transfer 400,0 g of sodium hydroxide (NaOH) into a plastic beaker with a lid and carefully add 500 ml of
water. Transfer the solution into a 1 000 ml volumetric plastic flask.
Dilute to the mark with water and mix.
5
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EN 14242:2023 (E)
5.15 Standard solutions
The standard solutions shall be traceable to international units mass or amount of substances i.e.
kilogram or mol. They should be prepared from pure metals or stoichiometric compounds.
Standard solutions containing sulphate ions shall not be used for the determination of elements which
form insoluble compounds with sulphate ions.
Standard solutions and calibration solutions with element concentrations ≤ 50 mg/l can be unstable and
shall be controlled before use.
NOTE 1 Calibration solutions can be prepared directly from standard solutions by weighing (see 8.6).
NOTE 2 For routine analysis, commercial standard solutions with stated traceability can also be used.
In the case of solution prepared before use and stored in appropriate receptacles, their concentration
shall either be controlled before use, or their stability over time be documented.
5.15.1 Antimony standard solution, 200 mg/l
Transfer 0,100 g of antimony (purity ≥ 99,99 % by mass) into a 250 ml beaker with a lid. Add 50 ml of
hydrochloric acid (5.9) and 2 ml of nitric acid (5.6), heat to complete the dissolution. Allow to cool.
Carefully add 50 ml of water and 50 ml of hydrochloric acid (5.9), transfer the solution quantitatively into
a 500 ml one-mark volumetric flask. Dilute to the mark with water and mix.
1 ml of this solution contains 200 µg of antimony.
5.15.2 Beryllium standard solution, 1 g/l
Transfer 1,000 g of beryllium (purity ≥ 99,99 % by mass) into a 400 ml beaker with a lid. Add 20 ml of
hydrochloric acid solution (5.10). Heat gently, if necessary, until the dissolution is complete, allow to cool
and transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the mark
with water and mix.
1 ml of this solution contains 1 mg of beryllium.
5.15.3 Bismuth standard solution, 1 g/l
Transfer 1,000 g of bismuth (purity ≥ 99,99 % by mass) into a 400 ml beaker with a lid. Add 18 ml of
hydrochloric acid (5.9), 6 ml of nitric acid (5.6) and 10 ml of water. Heat gently, if necessary, until the
dissolution is complete. Add 160 ml of hydrochloric acid solution (5.10), transfer the solution
quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the mark with water and mix.
1 ml of this solution contains 1 mg of bismuth.
5.15.4 Cadmium standard solution, 1 g/l
Transfer 1,000 g of cadmium (purity ≥ 99,99 % by mass) into a 400 ml beaker with a lid. Add of 10 ml of
water and 30 ml of nitric acid (5.6). Heat gently, if necessary, until the dissolution is complete, allow to
cool and transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the mark
with water and mix.
1 ml of this solution contains 1 mg of cadmium.
5.15.5 Calcium standard solution, 1 g/l
Transfer 2,497 3 g of calcium carbonate (purity ≥ 99,99 % by mass), previously dried at 200 °C to
constant mass into a 400 ml beaker with a lid. Dissolve in 40 ml of hydrochloric acid solution (5.10),
transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the mark with
water and mix.
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1 ml of this solution contains 1 mg of calcium.
5.15.6 Chromium standard solution, 1 g/l
5.15.6.1 Preparation using chromium metal
Transfer 0,5 g of chromium (purity ≥ 99,99 % by mass) into a 250 ml beaker with a lid. Add 40 ml of water
and 20 ml of hydrochloric acid (5.9). Heat gently, if necessary, until the dissolution is complete, allow to
cool and transfer the solution quantitatively into a 500 ml one-mark volumetric flask. Dilute to the mark
with water and mix.
1 ml of this solution contains 1 mg of chromium.
5.15.6.2 Preparation using potassium dichromate
Transfer 2,828 9 g of potassium dichromate (K Cr O ) previously dried at 130 °C to constant mass, into
2 2 7
a 400 ml beaker with a lid. Add 40 ml of water, 20 ml of hydrochloric acid solution (5.10) and dropwise
20 ml of hydrogen peroxide (5.13). Heat gently, without boiling, to evaporate the excess of hydrogen
peroxide. Allow to cool and transfer the solution quantitatively into a 1 000 ml volumetric flask. Dilute to
the mark with water and mix.
1 ml of this solution contains 1 mg of chromium.
5.15.7 Cobalt standard solution, 1 g/l
Transfer 1,000 g of cobalt (purity ≥ 99,99 % by mass) into a 400 ml beaker with a lid. Add 10 ml of water,
18 ml of hydrochloric acid (5.9) and 6 ml of nitric acid (5.6). Heat gently, if necessary, until the dissolution
is complete, allow to cool and transfer the solution quantitatively into a 1 000 ml one-mark volumetric
flask. Dilute to the mark with water and mix.
1 ml of this solution contains 1 mg of cobalt.
5.15.8 Copper standard solution, 1 g/l
Transfer 1,000 g of copper (purity ≥ 99,99 % by mass) into a 400 ml beaker with a lid. Add 40 ml of
hydrochloric acid solution (5.10) and stepwise 5 ml of hydrogen peroxide (5.13) while stirring. Heat until
the solution boils, allow to cool, transfer the solution quantitatively into a 1 000 ml one-mark volumetric
flask. Dilute to the mark with water and mix.
1 ml of this solution contains 1 mg of copper.
5.15.9 Gallium standard solution, 1 g/l
Transfer 1,000 g of gallium (purity ≥ 99,99 % by mass) into a 400 ml beaker with a lid. Add 10 ml of water
and 30 ml of nitric acid (5.6). Heat gently, if necessary, until the dissolution is complete, allow to cool and
transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the mark with
water and mix.
1 ml of this solution contains 1 mg of gallium.
5.15.10 Iron standard solution, 1 g/l
Transfer 1,000 g of iron (purity ≥ 99,99 % by mass) into a 400 ml beaker with a lid. Add 40 ml of
hydrochloric acid solution (5.10). Heat gently, if necessary, until the dissolution is complete, allow to cool
and transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the mark
with water and mix.
1 ml of this solution contains 1 mg of iron.
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5.15.11 Lead standard solution, 1 g/l
Transfer 1,000 g of lead (purity ≥ 99,99 % by mass), into a 250 ml beaker with a lid. Add 10 ml of water
and 10 ml of nitric acid solution (5.7). Heat gently, if necessary, until the dissolution is complete, then boil
until nitrous fumes have been expelled. Allow to cool and transfer the solution quantitatively into a
1 000 ml one-mark volumetric flask. Dilute to the mark with water and mix.
1 ml of this solution contains 1 mg of lead.
5.15.12 Lithium standard solution, 1 g/l
Transfer 5,324 0 g of lithium carbonate (purity ≥ 99,99 % by mass), previously dried at 200 °C to constant
mass into a 400 ml beaker with a lid. Dissolve in 40 ml hydrochloric acid solution (5.10), transfer the
solution quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the mark with water and mix.
1 ml of this solution contains 1 mg of lithium.
5.15.13 Magnesium standard solution, 1 g/l
Transfer 1,000 g of magnesium (purity ≥ 99,99 % by mass) into a 400 ml beaker with a lid. Add, by small
fractions, 40 ml of hydrochloric acid solution (5.10). Heat gently, if necessary, until the dissolution is
complete, allow to cool and transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask.
Dilute to the mark with water and mix.
1 ml of this solution contains 1 mg of magnesium.
5.15.14 Manganese standard solution, 1 g/l
The manganese (purity ≥ 99,99 % by mass) used to prepare the solution is released from superficial oxide
possibly present by introducing a few grams of metal in a 250 ml beaker containing 150 to 160 ml of
water and 15 to 20 ml of sulphuric acid (5.12). Shake and after a few seconds, allow the solution to settle
and add water. Repeat the water cleaning several times. Remove the metallic manganese and rinse with
acetone. Dry the metal in an oven at 100 °C for 2 minutes or with a hair dryer. Cool in a desiccator.
Transfer 1,000 g of manganese, precleaned as described above, into a 400 ml beaker with a lid. Add 40 ml
of hydrochloric acid solution (5.10). Heat gently, if necessary, until the dissolution is complete, allow to
cool, transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the mark
with water and mix.
1 ml of this solution contains 1 mg of manganese.
5.15.15 Nickel standard solution, 1 g/l
Transfer 1,000 g of nickel (purity ≥ 99,99 % by mass) into a 400 ml beaker with a lid. Add 40 ml of
hydrochloric acid solution (5.10). Heat gently, if necessary, until the dissolution is complete, allow to cool
and transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the mark
with water and mix.
1 ml of this solution contains 1 mg of nickel.
5.15.16 Sodium standard solution, 1 g/l
Transfer 2,305 1 g of sodium carbonate (purity ≥ 99,99 % by mass), previously dried at 200 °C to
constant mass into a 400 ml beaker with a lid. Dissolve in 40 ml of hydrochloric acid solution (5.10),
transfer the solution into a 1 000 ml volumetric flask. Dilute to the mark with water and mix.
1 ml of this solution contains 1 mg of sodium.
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5.15.17 Silicon standard solution, 100 mg/l
In a large platinum crucible with a lid, fuse 0,213 92 g of silica (SiO , purity ≥ 99,999 % by mass),
2
previously calcined at 1 000 °C to constant mass, with 2 g of a mixture of equal parts of sodium carbonate
(5.2) and potassium carbonate (5.3). Continue the fusion until a clear melt is obtained. Allow to cool,
transfer the melt into a 600 ml PTFE beaker with a lid, dissolve the fused mass with 400 ml of water. Heat
gently until the dissolution is complete. Slowly add 40 ml of nitric acid (5.6), while stirring strongly if
possible by means of a magnetic stirrer. Transfer the solution quantitatively into a 1 000 ml one-mark
volumetric flask, dilute to the mark with water and mix.
1 ml of this solution contains 100 µg of silicon.
NOTE This solution can be used for about 2 weeks.
5.15.18 Strontium standard solution, 1 g/l
Transfer 1,685 0 g of strontium carbonate (purity ≥ 99,99 % by mass), previously dried at 150 °C to
constant mass into a 400 ml beaker with a lid. Dissolve in 40 ml of hydrochloric acid solution (5.10),
transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the mark with
water and mix.
1 ml of this solution contains 1 mg of strontium.
5.15.19 Tin standard solution, 500 mg/l
Transfer 0,500 g of tin (purity ≥ 99,99 % by mass) into a 400 ml beaker with a lid. Add 100 ml of
hydrochloric acid (5.9). Heat gently until the dissolution is complete, allow to cool and transfer the
solution quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the mark with water and mix.
1 ml of this solution contains 500 µg of tin.
5.15.20 Titanium standard solution, 1 g/l
Transfer 0,200 g of titanium (purity ≥ 99,99 % by mass) into a 250 ml beaker with a lid. Add 50 ml of
hydrochloric acid solution (5.10) and 5 drops of hydrofluoric acid (5.11). Heat gently, if necessary, until
the dissolution is complete, allow to cool and transfer the solution quantitatively into a 200 ml one-mark
volumetric flask. Dilute to the mark with water and mix.
1 ml of this solution contains 1 mg of titanium.
5.15.21 Vanadium standard solution, 1 g/l
Transfer 0,5 g of vanadium (purity ≥ 99,99 % by mass) into a 250 ml beaker with a lid. Add 30 ml of
hydrochloric acid (5.9) and 10 ml of nitric acid (5.6). Heat gently, if necessary, until the dissolution is
complete, allow to cool and transfer the solution quantitatively into a 500 ml one-mark volumetric flask.
Dilute to the mark with water and mix.
1 ml of this solution contains 1 mg of vanadium.
5.15.22 Zinc standard solution, 1 g/l
Transfer 1,000 g of zinc (purity ≥ 99,99 % by mass) into a 400 ml beaker with a lid. Add 40 ml of
hydrochloric acid solution (5.10). Heat gently, if necessary, until the dissolution is complete, allow to cool
and transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the mark
with water and mix.
1 ml of this solution contains 1 mg of zinc.
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EN 14242:2023 (E)
5.15.23 Zirconium standard solution, 1 g/l
In a large platinum crucible with a lid, fuse 1,350 8 g of zirconium dioxide ZrO , (purity ≥ 99,99 % by
2
mass), previously calcined at 1 000 °C to constant mass, with 10 g of potassium disulphate (5.5). After
cooling, dissolve the fused product with 25 ml of hydrochloric acid solution (5.10). Transfer the solution
quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the mark with water and mix.
1 ml of this solution contains 1 mg of zirconium.
5.16 Internal reference element solutions
5.16.1 Lanthanum solution, 1 g/l
Transfer 1,173 g of lanthanum oxide La O (purity ≥ 99,99 %, by mass), previously dried at 150 °C to
2 3
constant mass, into a 400 ml beaker with a lid. Dissolve in 40 ml of hydrochloric acid solution (5.10),
transfer the solution into a 1 000 ml volumetric flask, dilute to the mark with water and mix.
5.16.2 Lanthanum solution, 200 mg/l
Transfer 20,0 ml of the lanthanum solution (5.16.1) into a 100 ml volumetric flask, add 1 ml of
hydrochloric acid solution (5.10), dilute to the mark with water and mix.
5.16.3 Scandium solution, 0,1 g/l
Transfer 100,0 mg of scandium (purity ≥ 99,99 %, by mass) into a 400 ml beaker with a lid. Add 20 ml of
hydrochloric acid solution (5.10). Heat gently, if necessary, until the dissolution is complete. Allow to cool,
transfer the solution into a 1 000 ml volumetric flask, dilute to the mark with water and mix.
NOTE Scandium solutions can be unstable.
5.16.4 Scandium solution, 20 mg/l
Transfer 20,0 ml of the scandium solution (5.16.3) into a 100 ml volumetric flask, add 1 ml of
hydrochloric acid solution (5.10), dilute to the mark with water and mix.
5.16.5 Molybdenum solution, 1 g/l
Dissolve 1,84 g of ammonium molybdate (NH ) Mo O × 4H O into a 1 000 ml volumetric flask with
4 6 7 24 2
water. Dilute to the mark with water and mix.
5.16.6 Molybdenum solution, 200 mg/l
Transfer 20,0 ml of the molybdenum solution (5.16.5) into a 100 ml volumetric flask, add 1 ml of
hydrochloric acid solution (5.10), dilute to the mark with water and mix.
6 Apparatus
All volumetric glassware shall be class A and calibrated in accordance with EN ISO 648 or EN ISO 1042,
as appropriate.
Ordinary laboratory equipment can be the following.
6.1 Optical emission spectrometer, equipped with inductively coupled plasma.
This shall be equipped with a nebulization system. The instrument used will be satisfactory if, after
optimizing in accordance with the manufacturer’s instructions, it meets the performance criteria given
in Annex B.
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SIST EN 1424
...
SLOVENSKI STANDARD
oSIST prEN 14242:2022
01-marec-2022
Aluminij in aluminijeve zlitine - Kemična analiza - Analiza s spektrometrijo optične
emisije z induktivno sklopljeno plazmo
Aluminium and aluminium alloys - Chemical analysis - Inductively coupled plasma optical
emission spectral analysis
Aluminium und Aluminiumlegierungen - Chemische Analyse - Optische
Emissionspektralanalyse mit induktiv gekoppelter Plasmaanregung
Aluminium et alliages d'aluminium - Analyse chimique - Analyse par spectrométrie
d'émission optique en plasma induit
Ta slovenski standard je istoveten z: prEN 14242
ICS:
77.040.30 Kemijska analiza kovin Chemical analysis of metals
77.120.10 Aluminij in aluminijeve zlitine Aluminium and aluminium
alloys
oSIST prEN 14242:2022 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN 14242:2022
DRAFT
EUROPEAN STANDARD
prEN 14242
NORME EUROPÉENNE
EUROPÄISCHE NORM
January 2022
ICS 77.040.30; 77.120.10 Will supersede EN 14242:2004
English Version
Aluminium and aluminium alloys - Chemical analysis -
Inductively coupled plasma optical emission spectral
analysis
Aluminium et alliages d'aluminium - Analyse chimique Aluminium und Aluminiumlegierungen - Chemische
- Analyse par spectrométrie d'émission optique en Analyse - Optische Emissionspektralanalyse mit
plasma induit induktiv gekoppelter Plasmaanregung
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee
CEN/TC 132.
If this draft becomes a European Standard, CEN members are bound to comply with the CEN/CENELEC Internal Regulations
which stipulate the conditions for giving this European Standard the status of a national standard without any alteration.
This draft European Standard was established by CEN in three official versions (English, French, German). A version in any other
language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC
Management Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.
Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are
aware and to provide supporting documentation.
Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without
notice and shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 14242:2022 E
worldwide for CEN national Members.
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Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 4
5 Reagents . 5
6 Apparatus . 11
7 Sampling . 11
8 Procedure. 12
9 Correction of short-term fluctuations and drift . 15
10 Investigation of interferences . 16
11 Expression of the results . 16
12 Test report . 17
Annex A (informative) Analytical wavelengths . 18
Annex B (informative) Plasma optical emission spectrometer — Suggested performance
criteria to be checked . 20
B.1 Short and long term stability . 20
B.2 Evaluating the background equivalent concentration . 20
B.3 Evaluating the limit of detection . 21
B.4 Linearity of the calibration curves . 21
Bibliography . 22
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European foreword
This document (prEN 14242:2022) has been prepared by Technical Committee CEN/TC 132 “Aluminium
and aluminium alloys”, the secretariat of which is held by AFNOR.
This document is currently submitted to the CEN Enquiry.
This document will supersede EN 14242:2002.
In comparison with the previous edition, the following technical modifications have been made:
— Modification of the scope;
— New subclause 5.15.6;
— Several editorial modifications.
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1 Scope
This document specifies an inductively coupled plasma optical emission spectrometric method
(ICP-OES) for the analysis of aluminium and aluminium alloys.
This method is applicable to the determination of silicon, iron, copper, manganese, magnesium,
chromium, nickel, zinc, titanium, gallium, vanadium, beryllium, bismuth, calcium, cadmium, cobalt,
lithium, sodium, lead, antimony, tin, strontium and zirconium in aluminium and aluminium alloys.
The content of the elements to be determined should be at least 10 times higher than the detection limits
of the method.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
EN 12258-2:2001, Aluminium and aluminium alloys — Terms and definitions — Part 2: Chemical analysis
EN 14361, Aluminium and aluminium alloys - Chemical analysis - Sampling from metal melts
EN ISO 648, Laboratory glassware - Single-volume pipettes (ISO 648)
EN ISO 1042, Laboratory glassware - One-mark volumetric flasks (ISO 1042)
EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696)
3 Terms and definitions
For the purposes of this document, the terms and definitions given in EN 12258-2:2001 apply.
4 Principle
A test portion is dissolved with:
— a sodium hydroxide solution followed by acidification with a mixture of nitric acid and hydrochloric
acid; or
— nitric acid and hydrofluoric acid; or
— a mixture of hydrochloric acid and nitric acid; or
— hydrochloric acid and hydrogen peroxide,
according to the alloy type and the element to be determined.
After suitable dilution and, if necessary, addition of an internal reference element, nebulisation of the
solution into an inductively coupled plasma emission spectrometer and measurement of the intensity of
the emitted light (including, where appropriate, that of the internal reference element).
The emission signals on the selected analytical lines (see Annex A) are then compared with those of the
calibration solutions.
NOTE 1 The ranges of application and the accuracy of the method or any alternative steps is validated by the
laboratory. Approximate ranges of application are given in Annex A.
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NOTE 2 All instrumentation, including software used in the laboratories, are different and subject to change.
Therefore, only general criteria for calibration and measurement are specified.
5 Reagents
During the analysis, unless otherwise specified, use only reagents of recognized analytical grade and only
grade 2 water as specified in EN ISO 3696.
The same reagents should be used for the preparation of calibration solutions and of sample solutions.
5.1 Aluminium, purity ≥ 99,999 % by mass.
5.2 Sodium carbonate (Na CO )
2 3
5.3 Potassium carbonate (K CO )
2 3
5.4 Sodium nitrite (NaNO )
2
5.5 Potassium disulphate (K S O )
2 2 7
5.6 Nitric acid, ρ = 1,40 g/ml approximately.
5.7 Nitric acid solution, 1 + 1
Carefully add 500 ml of nitric acid (5.6) to 400 ml water, allow to cool, dilute to 1 l with water and mix.
5.8 Nitric acid solution, 4 mol/l
Carefully add 27,7 ml of nitric acid (5.6) to 50 ml water, allow to cool, dilute to 100 ml with water and
mix.
5.9 Hydrochloric acid, ρ = 1,19 g/ml, approximately
5.10 Hydrochloric acid solution, 1 + 1
Carefully add 500 ml of hydrochloric acid (5.9) to 400 ml water, allow to cool, dilute to 1 l with water and
mix.
5.11 Hydrofluoric acid, ρ = 1,14 g/ml, approximately.
5.12 Sulphuric acid, ρ = 1,84 g/ml approximately.
5.13 Hydrogen peroxide, 30 % (mass fraction) solution.
5.14 Sodium hydroxide solution, 400 g/l
Transfer 400,0 g of sodium hydroxide (NaOH) into a plastic beaker with a lid and carefully add 500 ml of
water. Transfer the solution into a 1 000 ml volumetric plastic flask.
Dilute to the mark with water and mix.
5
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5.15 Standard solutions
The standard solutions shall be traceable to international units mass or amount of substances i.e.
kilogram or mol. They should be prepared from pure metals or stoichiometric compounds.
Standard solutions containing sulphate ions shall not be used for the determination of elements which
form insoluble compounds with sulphate ions.
Standard solutions and calibration solutions with element concentrations ≤ 50 mg/l can be unstable and
shall be prepared just before use.
NOTE 1 Calibration solutions can be prepared directly from standard solutions by weighting (see 8.6).
NOTE 2 For routine analysis, commercial standard solutions with stated traceability can also be used.
5.15.1 Antimony standard solution, 200 mg/l
Transfer 0,100 g of antimony (purity ≥ 99,99 % by mass) into a 250 ml beaker with a lid. Add 50 ml of
hydrochloric acid (5.9) and 2 ml of nitric acid (5.6), heat to complete the dissolution. Allow to cool.
Carefully add 50 ml of water and 50 ml of hydrochloric acid (5.9), transfer the solution quantitatively into
a 500 ml one-mark volumetric flask. Dilute to the volume with water and mix.
1 ml of this solution contains 200 µg of antimony.
5.15.2 Beryllium standard solution, 1 g/l
Transfer 1,000 g of beryllium (purity ≥ 99,99 % by mass) into a 400 ml beaker with a lid. Add 20 ml of
hydrochloric acid solution (5.10). Heat gently, if necessary, until the dissolution is complete, allow to cool
and transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the volume
with water and mix.
1 ml of this solution contains 1 mg of beryllium.
5.15.3 Bismuth standard solution, 1 g/l
Transfer 1,000 g of bismuth (purity ≥ 99,99 % by mass) into a 400 ml beaker with a lid. Add 18 ml of
hydrochloric acid (5.9), 6 ml of nitric acid (5.6) and 10 ml of water. Heat gently, if necessary, until the
dissolution is complete. Add 160 ml of hydrochloric acid solution (5.10), transfer the solution
quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the volume with water and mix.
1 ml of this solution contains 1 mg of bismuth.
5.15.4 Cadmium standard solution, 1 g/l
Transfer 1,000 g of cadmium (purity ≥ 99,99 % by mass) to a 400 ml beaker with a lid. Add of 10 ml of
water and 30 ml of nitric acid (5.6). Heat gently, if necessary, until the dissolution is complete, allow to
cool and transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the
volume with water and mix.
1 ml of this solution contains 1 mg of cadmium.
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5.15.5 Calcium standard solution, 1 g/l
Transfer 2,4973 g of calcium carbonate (purity ≥ 99,99 % by mass), previously dried at 200 °C to constant
mass into a 400 ml beaker with a lid. Dissolve in 40 ml of hydrochloric acid solution (5.10), transfer the
solution quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the volume with water and
mix.
1 ml of this solution contains 1 mg of calcium.
5.15.6 Chromium standard solution, 1 g/l
5.15.6.1 Preparation using chromium metal
Transfer 0,5 g of chromium (purity ≥ 99,99 % by mass) into a 250 ml beaker with a lid. Add 40 ml of water
and 20 ml of hydrochloric acid (5.9). Heat gently, if necessary, until the dissolution is complete, allow to
cool and transfer the solution quantitatively into a 500 ml one-mark volumetric flask. Dilute to the
volume with water and mix.
1 ml of this solution contains 1 mg of chromium.
5.15.6.2 Preparation using potassium dichromate
Transfer 2,828 9 g of potassium dichromate (K Cr O ) previously dried at 130 °C to constant mass, into a
2 2 7
400 ml beaker with a lid. Add 40 ml of water, 20 ml of hydrochloric acid solution (5.10) and dropwise
20 ml of hydrogen peroxide (5.13). Heat gently, without boiling, to evaporate the excess of hydrogen
peroxide. Allow to cool and transfer the solution quantitatively into a 1 000 ml volumetric flask. Dilute to
the volume with water and mix.
1 ml of this solution contains 1 mg of chromium.
5.15.7 Cobalt standard solution, 1 g/l
Transfer 1,000 g of cobalt (purity ≥ 99,99 % by mass) into a 400 ml beaker with a lid. Add 10 ml of water,
18 ml of hydrochloric acid (5.9) and 6 ml of nitric acid (5.6). Heat gently, if necessary, until the dissolution
is complete, allow to cool and transfer the solution quantitatively into a 1 000 ml one-mark volumetric
flask. Dilute to the volume with water and mix.
1 ml of this solution contains 1 mg of cobalt.
5.15.8 Copper standard solution, 1 g/l
Transfer 1,000 g of copper (purity ≥ 99,99 % by mass) into a 400 ml beaker with a lid. Add 40 ml of
hydrochloric acid solution (5.10) and stepwise 5 ml of hydrogen peroxide (5.13) while stirring. Heat until
the solution boils, allow to cool, transfer the solution quantitatively into a 1 000 ml one-mark volumetric
flask. Dilute to the volume with water and mix.
1 ml of this solution contains 1 mg of copper.
5.15.9 Gallium standard solution, 1 g/l
Transfer 1,000 g of gallium (purity ≥ 99,99 % by mass) into a 400 ml beaker with a lid. Add 10 ml of water
and 30 ml of nitric acid (5.6). Heat gently, if necessary, until the dissolution is complete, allow to cool and
transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the volume with
water and mix.
1 ml of this solution contains 1 mg of gallium.
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5.15.10 Iron standard solution, 1 g/l
Transfer 1,000 g of iron (purity ≥ 99,99 % by mass) into a 400 ml beaker with a lid. Add 40 ml of
hydrochloric acid solution (5.10). Heat gently, if necessary, until the dissolution is complete, allow to cool
and transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the volume
with water and mix.
1 ml of this solution contains 1 mg of iron.
5.15.11 Lead standard solution, 1 g/l
Transfer 1,000 g of lead (purity ≥ 99,99 % by mass), into a 250 ml beaker with a lid. Add 10 ml of water
and 10 ml of nitric acid solution (5.7). Heat gently, if necessary, until the dissolution is complete, then boil
until nitrous fumes have been expelled. Allow to cool and transfer the solution quantitatively into a
1 000 ml one-mark volumetric flask. Dilute to the volume with water and mix.
1 ml of this solution contains 1 mg of lead.
5.15.12 Lithium standard solution, 1 g/l
Transfer 5,3240 g of lithium carbonate (purity ≥ 99,99 % by mass), previously dried at 200 °C to constant
mass into a 400 ml beaker with a lid. Dissolve in 40 ml hydrochloric acid solution (5.10), transfer the
solution quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the volume with water and
mix.
1 ml of this solution contains 1 mg of lithium.
5.15.13 Magnesium standard solution, 1 g/l
Transfer 1,000 g of magnesium (purity ≥ 99,99 % by mass) into a 400 ml beaker with a lid. Add, by small
fractions, 40 ml of hydrochloric acid solution (5.10). Heat gently, if necessary, until the dissolution is
complete, allow to cool and transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask.
Dilute to the volume with water and mix.
1 ml of this solution contains 1 mg of magnesium.
5.15.14 Manganese standard solution, 1 g/l
The manganese (purity ≥ 99,99 % by mass) used to prepare the solution is released from superficial oxide
possibly present by introducing a few grams of metal in a 250 ml beaker containing 150 to 160 ml of
water and 15 to 20 ml of sulphuric acid (5.12). Shake and after a few seconds, allow the solution to settle
and add water. Repeat the water cleaning several times. Remove the metallic manganese and rinse with
acetone. Dry the metal in an oven at 100 °C for 2 minutes or with a hair dryer. Cool in a desiccator.
Transfer 1,000 g of manganese, precleaned as described above, into a 400 ml beaker with a lid. Add 40 ml
of hydrochloric acid solution (5.10). Heat gently, if necessary, until the dissolution is complete, allow to
cool, transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the volume
with water and mix.
1 ml of this solution contains 1 mg of manganese.
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5.15.15 Nickel standard solution, 1 g/l
Transfer 1,000 g of nickel (purity ≥ 99,99 % by mass) into a 400 ml beaker with a lid. Add 40 ml of
hydrochloric acid solution (5.10). Heat gently, if necessary, until the dissolution is complete, allow to cool
and transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the volume
with water and mix.
1 ml of this solution contains 1 mg of nickel.
5.15.16 Sodium standard solution, 1 g/l
Transfer 2,3051 g of sodium carbonate (purity ≥ 99,99 % by mass), previously dried at 200 °C to constant
mass into a 400 ml beaker with a lid. Dissolve in 40 ml of hydrochloric acid solution (5.10), transfer the
solution to a 1 000 ml volumetric flask. Dilute to the volume with water and mix.
1 ml of this solution contains 1 mg of sodium.
5.15.17 Silicon standard solution, 100 mg/l
In a large platinum crucible with a lid, decompose 0,2139 2 g of pure silica (SiO , purity ≥ 99,999 % by
2
mass), previously calcined at 1 000 °C to constant mass, with 2 g of a mixture of equal parts of sodium
carbonate (5.2) and potassium carbonate (5.3). Continue the fusion until a clear melt is obtained. Allow
to cool, transfer the melt to a 600 ml PTFE beaker with a lid, dissolve the fused mass with 400 ml of water.
Heat gently until the dissolution is complete. Slowly add 40 ml of nitric acid (5.6), while stirring strongly
if possible by means of a magnetic stirrer. Transfer the solution quantitatively into a 1 000 ml one-mark
volumetric flask, dilute to the volume with water and mix.
1 ml of this solution contains 100 µg of silicon.
NOTE This solution can be used for about two weeks.
5.15.18 Strontium standard solution, 1 g/l
Transfer 1,685 0 g of strontium carbonate (purity ≥ 99,99 % by mass), previously dried at 150 °C to
constant mass into a 400 ml beaker with a lid. Dissolve in 40 ml of hydrochloric acid solution (5.10),
transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the volume with
water and mix.
1 ml of this solution contains 1 mg of strontium.
5.15.19 Tin standard solution, 500 mg/l
Transfer 0,500 g of tin (purity ≥ 99,99 % by mass) into a 400 ml beaker with a lid. Add 100 ml of
hydrochloric acid (5.9). Heat gently until the dissolution is complete, allow to cool and transfer the
solution quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the volume with water and
mix.
1 ml of this solution contains 500 µg of tin.
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5.15.20 Titanium standard solution, 1 g/l
Transfer 0,200 g of titanium (purity ≥ 99,99 % by mass) into a 250 ml beaker with a lid. Add 50 ml of
hydrochloric acid solution (5.10) and 5 drops of hydrofluoric acid (5.11). Heat gently, if necessary, until
the dissolution is complete, allow to cool and transfer the solution quantitatively into a 200 ml one-mark
volumetric flask. Dilute to the volume with water and mix.
1 ml of this solution contains 1 mg of titanium.
5.15.21 Vanadium standard solution, 1 g/l
Transfer 0,5 g of vanadium (purity ≥ 99,99 % by mass) into a 250 ml beaker with a lid. Add 30 ml of
hydrochloric acid (5.9) and 10 ml of nitric acid (5.6). Heat gently, if necessary, until the dissolution is
complete, allow to cool and transfer the solution quantitatively into a 500 ml one-mark volumetric flask.
Dilute to the volume with water and mix.
1 ml of this solution contains 1 mg of vanadium.
5.15.22 Zinc standard solution, 1 g/l
Transfer 1,000 g of zinc (purity ≥ 99,99 % by mass) into a 400 ml beaker with a lid. Add 40 ml of
hydrochloric acid solution (5.10). Heat gently, if necessary, until the dissolution is complete, allow to cool
and transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the volume
with water and mix.
1 ml of this solution contains 1 mg of zinc.
5.15.23 Zirconium standard solution, 1 g/l
In a large platinum crucible with a lid, fuse 1,3508 g of zirconium dioxide ZrO , (purity ≥ 99,99 % by
2
mass), previously calcined at 1 000 °C to constant mass, with 10 g of potassium disulphate (5.5). After
cooling dissolve the fused mass with 25 ml of hydrochloric acid solution (5.10). Transfer the solution
quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the volume with water and mix.
1 ml of this solution contains 1 mg of zirconium.
5.16 Internal reference element solutions
5.16.1 Lanthanum solution, 1 g/l
O (purity ≥ 99,99 %, by mass), previously dried at 150 °C to
Transfer 1,173 g of lanthanum oxide La2 3
constant mass, into a 400 ml beaker with a lid. Add 40 ml of hydrochloric acid solution (5.10), transfer
the solution into a 1 000 ml volumetric flask, dilute to the volume with water and mix.
5.16.2 Lanthanum solution, 200 mg/l
Transfer 20,0 ml of the lanthanum solution (5.16.1) into a 100 ml volumetric flask, add 1 ml of
hydrochloric acid solution (5.10), dilute to the volume with water and mix.
5.16.3 Scandium solution, 0,1 g/l
Transfer 100,0 mg of scandium (purity ≥ 99,99 %, by mass) into a 400 ml beaker with a lid. Add 20 ml of
hydrochloric acid solution (5.10). Heat gently, if necessary, until the dissolution is complete. Allow to cool,
transfer the solution into a 1 000 ml volumetric flask, dilute to the volume with water and mix.
NOTE Scandium solutions can be unstable.
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5.16.4 Scandium solution, 20 mg/l
Transfer 20,0 ml of the scandium solution (5.16.3) into a 100 ml volumetric flask, add 1 ml of
hydrochloric acid solution (5.10), dilute to the volume with water and mix.
5.16.5 Molybdenum solution, 1 g/l
Dissolve 1,84 g of ammonium molybdate (NH ) Mo O × 4H O into a 1 000 ml volumetric flask with
4 6 7 24 2
water. Dilute to the volume with water and mix.
5.16.6 Molybdenum solution, 200 mg/l
Transfer 20,0 ml of the molybdenum solution (5.16.5) into a 100 ml volumetric flask, add 1 ml of
hydrochloric acid solution (5.10), dilute to the volume with water and mix.
6 Apparatus
All volumetric glassware shall be class A and calibrated in accordance with EN ISO 648 or EN ISO 1042,
as appropriate.
Ordinary laboratory equipment and the following.
6.1 Optical emission spectrometer, equipped with inductively coupled plasma.
This shall be equipped with a nebulization system. The instrument used will be satisfactory if, after
optimizing in accordance with the manufacturer’s instructions, it meets the performance criteria given
in Annex B.
The spectrometer can be either a simultaneous or a sequential one (for analytical lines, see Annex A). If a
sequential spectrometer can be equipped with an extra arrangement for simultaneous measurement of
the internal reference element line, it can be used with the internal reference method. If the sequential
spectrometer is not equipped with this arrangement, an internal reference cannot be used and an
alternative measurement technique without internal reference element shall be used.
For solutions containing hydrofluoric acid the instrument shall be equipped with a fluoride-resistant
nebulizer.
The nebulizer should be selected carefully. Many of the available fluoride-resistant nebulizers are not as
stable as the glass nebulizers.
6.2 PTFE-beakers, 400 ml, with lid.
6.3 Platinum crucibles, 100 ml to 120 ml, with a lid.
6.4 Plastic bottles, approximately 100 ml, with small neck and cap.
The plastic equipment should be selected carefully to avoid losses and contaminations.
7 Sampling
7.1 General
Sampling from aluminium melts shall be carried out in accordance with EN 14361.
The analytical result should represent the average chemical composition of a test sample, a laboratory
sample or an inspection lot.
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7.2 Test sample
The test sample is normally in the form of millings or drillings.
If the chemical composition of the test sample is thought to be not uniform, e.g. in case of unwrought
products, its preparation shall follow a documented procedure to ensure the required representativity.
If necessary, e.g. for the determination of low contents of alkaline or alkaline earth elements, the test
sample should be cleaned in accordance with a suitable procedure (solution, temperature and time). The
cleaning procedure shall be adapted to the alloy, analytes and the content to be determined.
The test sample should be sufficiently homogeneous for the quantity of the test portion.
8 Procedure
8.1 Test portion
Weigh, to the nearest 0,001 g, about 0,5 g of the test sample.
8.2 Dissolution procedure I with sodium hydroxide solution
8.2.1 This procedure is applicable for the determination of silicon, iron, copper, manganese,
magnesium, chromium, nickel, zinc, titanium, vanadium, beryllium, cadmium, cobalt, lead, antimony, tin,
strontium and zirconium in aluminium and aluminium alloys.
8.2.2 Transfer the test portion (8.1) into a 400 ml PTFE-beaker with a lid (6.2) or into a platinum
crucible with a lid (6.3).
8.2.3 Cover the test portion with water. Add 6 ml of sodium hydroxide solution (5.14) using a plastic
pipette. After the dissolution reaction ceases, add 1 ml hydrogen peroxide (5.13). Heat gently until the
dissolution is complete.
8.2.4 If the silicon content of the test sample is more than 0,5 % by mass carefully evaporate to a syrupy
consistency. Allow to cool a little, carefully add 30 ml of water and heat gently until the dissolution is
complete. If a platinum crucible (6.3) has been used, transfer the solution quantitatively into a 400 ml
PTFE-beaker, containing 25 ml of nitric acid solution (5.7) and 10 ml of hydrochloric acid sol
...
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