SIST-TS CEN/TS 15605:2008
(Main)Copper and copper alloys - Inductively coupled plasma optical emission spectral analysis
Copper and copper alloys - Inductively coupled plasma optical emission spectral analysis
This document specifies seven inductively coupled plasma emission spectrometry methods (A to G) for the determination of alloying elements and impurities in copper and copper alloys in the form of unwrought, wrought and cast products.
These methods are applicable to the elements listed in Tables 1 to 7 within the composition ranges shown:
Table 1 - Coppers
Table 2 - Copper-zinc alloys
Table 3 - Copper-tin alloys
Table 4 - Copper-aluminium alloys
Table 5 - Copper-beryllium alloys
Table 6 - Copper-nickel alloys
Table 7 - Copper-tin-lead alloys
NOTE 1 The ranges specified for each method can be extended or adapted, for the determination of lower mass frac-tions.
NOTE 2 Other elements may be included. However such elements and their mass fractions should be carefully checked, taking into account interference, sensitivity, resolution and linearity criteria for each instrument and each wave-length.
Kupfer und Kupferlegierungen - Optische Emissionsspektralanalyse mit induktiv gekoppelter Plasmaanregung
Cuivre et alliages de cuivre - Analyse par spectrométrie d'émission optique avec source a plasma induit par haute fréquence
Le présent document spécifie sept méthodes de spectrométrie d'émission avec plasma induit par haute fréquence (A à G) pour la détermination des éléments d'alliage et des impuretés dans le cuivre et les alliages de cuivre sous la forme de produits non corroyés, corroyés et moulés.
Ces méthodes sont applicables aux éléments énumérés dans les Tableaux 1 à 7 dans les domaines de composition indiqués :
Baker in bakrove zlitine - Analiza s spektrometrijo optične emisije z induktivno sklopljeno plazmo
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST-TS CEN/TS 15605:2008
01-januar-2008
%DNHULQEDNURYH]OLWLQH$QDOL]DVVSHNWURPHWULMRRSWLþQHHPLVLMH]LQGXNWLYQR
VNORSOMHQRSOD]PR
Copper and copper alloys - Inductively coupled plasma optical emission spectral analysis
Kupfer und Kupferlegierungen - Optische Emissionsspektralanalyse mit induktiv
gekoppelter Plasmaanregung
Cuivre et alliages de cuivre - Analyse par spectrométrie d'émission optique avec source
a plasma induit par haute fréquence
Ta slovenski standard je istoveten z: CEN/TS 15605:2007
ICS:
77.120.30 Baker in bakrove zlitine Copper and copper alloys
SIST-TS CEN/TS 15605:2008 en,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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TECHNICAL SPECIFICATION
CEN/TS 15605
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
November 2007
ICS 77.120.30
English Version
Copper and copper alloys - Inductively coupled plasma optical
emission spectrometry
Cuivre et alliages de cuivre - Analyse par spectrométrie Kupfer und Kupferlegierungen - Optische
d'émission optique avec source à plasma induit par haute Emissionsspektrometrie mit induktiv gekoppelter
fréquence Plasmaanregung
This Technical Specification (CEN/TS) was approved by CEN on 21 October 2007 for provisional application.
The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to submit their
comments, particularly on the question whether the CEN/TS can be converted into a European Standard.
CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS available
promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the CEN/TS)
until the final decision about the possible conversion of the CEN/TS into an EN is reached.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,
Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36 B-1050 Brussels
© 2007 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 15605:2007: E
worldwide for CEN national Members.
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CEN/TS 15605:2007 (E)
Contents Page
Foreword.3
1 Scope .4
2 Normative references .6
3 Principle.7
4 Reagents and materials .7
5 Apparatus .11
6 Sampling.12
7 Procedure .12
8 Expression of results .40
9 Precision.40
10 Test report .44
Annex A (informative) Optical emission spectrometer (OES) — Suggested performance criteria to
be checked .45
Bibliography .47
2
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CEN/TS 15605:2007 (E)
Foreword
This document (CEN/TS 15605:2007) has been prepared by Technical Committee CEN/TC 133 “Copper and
copper alloys”, the secretariat of which is held by DIN.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
Within its programme of work, Technical Committee CEN/TC 133 requested CEN/TC 133/WG 10 "Methods of
Analysis" to prepare the following Technical Specification:
CEN/TS 15605, Copper and copper alloys — Inductively coupled plasma optical emission spectrometry
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to announce this Technical Specification: Austria, Belgium, Bulgaria, Cyprus, Czech Re-
public, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithua-
nia, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Swe-
den, Switzerland and the United Kingdom.
3
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CEN/TS 15605:2007 (E)
1 Scope
This document specifies seven inductively coupled plasma emission spectrometry methods (A to G) for the
determination of alloying elements and impurities in copper and copper alloys in the form of unwrought,
wrought and cast products.
These methods are applicable to the elements listed in Tables 1 to 7 within the composition ranges shown:
Table 1 — Coppers
Mass fraction %
Element
min. max.
Sn 0,02 0,60
Pb 0,02 0,60
Zn 0,02 0,60
Fe 0,01 0,60
Ni 0,01 0,60
Mn 0,01 0,60
Al 0,02 0,60
P 0,01 0,40
Be 0,01 0,60
Co 0,01 0,60
Cd 0,01 0,60
Table 2 — Copper-zinc alloys
Mass fraction %
Element
min. max.
Sn 0,05 2,00
Pb 0,03 4,00
Zn 10,00 42,00
Fe 0,01 5,00
Ni 0,02 4,00
Mn 0,01 6,00
P 0,01 0,40
Al 0,02 9,00
As 0,01 0,20
4
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CEN/TS 15605:2007 (E)
Table 3 — Copper-tin alloys
Mass fraction %
Element
min. max.
Sn 3,00 16,00
Pb 0,01 9,00
Zn 0,03 6,00
Fe 0,01 1,00
Ni 0,05 7,00
Mn 0,01 0,40
P 0,01 0,60
Al 0,01 0,50
Sb 0,02 1,60
As 0,02 0,25
Table 4 — Copper-aluminium alloys
Mass fraction %
Element
min. max.
Sn 0,02 0,50
Pb 0,03 0,50
Zn 0,03 1,00
Fe 0,05 7,00
Ni 0,10 8,00
Mn 0,01 5,00
Al 6,00 14,00
Cd 0,01 0,50
Mg 0,002 0,15
Table 5 — Copper-beryllium alloys
Mass fraction %
Element
min. max.
Sn 0,02 0,20
Pb 0,01 0,20
Zn 0,03 0,20
Fe 0,03 0,30
Ni 0,04 2,50
Mn 0,006 0,15
Al 0,03 0,20
Be 0,08 4,00
Co 0,03 4,00
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CEN/TS 15605:2007 (E)
Table 6 — Copper-nickel alloys
Mass fraction %
Element
min. max.
Sn 0,10 0,50
Pb 0,03 0,50
Zn 0,04 2,00
Fe 0,10 4,00
Ni 7,00 35,00
Mn 0,02 3,00
Al 0,02 0,50
Table 7 — Copper-tin-lead alloys
Mass fraction %
Element
min. max.
Sn 3,00 12,00
Pb 8,00 25,00
Zn 0,05 3,00
Fe 0,01 0,50
Ni 0,05 3,00
Mn 0,01 0,30
P 0,02 0,40
Al 0,01 0,40
Sb 0,02 0,80
NOTE 1 The ranges specified for each method can be extended or adapted, for the determination of lower mass frac-
tions.
NOTE 2 Other elements may be included. However such elements and their mass fractions should be carefully
checked, taking into account interference, sensitivity, resolution and linearity criteria for each instrument and each wave-
length.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated refer-
ences, only the edition cited applies. For undated references, the latest edition of the referenced document
(including any amendments) applies.
ISO 1811-1, Copper and copper alloys — Selection and preparation of samples for chemical analysis —
Part 1: Sampling of cast unwrought products
ISO 1811-2, Copper and copper alloys — Selection and preparation of samples for chemical analysis —
Part 2: Sampling of wrought products and castings
NOTE Informative references to documents used in the preparation of this Technical Specification, and cited at the
appropriate places in the text, are listed in the Bibliography.
6
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CEN/TS 15605:2007 (E)
3 Principle
Dissolution of a test portion with hydrochloric and nitric acid. After suitable dilution and addition of an internal
reference element, nebulization of the solution into an inductively coupled plasma emission spectrometer and
measurement of the intensity of the emitted light, including that of the internal reference element.
4 Reagents and materials
During the analysis, use only reagents of recognised analytical grade and only distilled water or water of
equivalent purity.
The same reagents should be used for the preparation of calibration solutions and of sample solutions.
4.1 Hydrochloric acid, HCl (ρ = 1,19 g/ml).
4.2 Hydrochloric acid, solution 1 + 1
Dilute 500 ml of hydrochloric acid (4.1) with 500 ml of water.
4.3 Nitric acid, HNO (ρ = 1,40 g/ml).
3
4.4 Nitric acid, solution 1 + 1
Dilute 500 ml of nitric acid (4.3) with 500 ml of water.
4.5 Hydrofluoric acid, HF (ρ = 1,13 g/ml).
4.6 Sulphuric acid, H SO (4,5 mol/l).
2 4
4.7 Electrolytic copper.
4.8 Zinc granules of 99,999 % purity.
4.9 Aluminium stock solution, 10 g/l Al
Weigh (5 ± 0,001) g of pure aluminium (Al 99,99 % mass fraction), transfer into a 600 ml beaker and cover
with a watch glass. Dissolve it in 250 ml hydrochloric acid solution (4.2). After cooling, transfer the solution
quantitatively into a 500 ml one-mark volumetric flask, dilute to the mark with water and mix well.
1 ml of this solution contains 10 mg of Al.
4.10 Aluminium stock solution, 1 g/l Al
Weigh (1 ± 0,001) g of pure aluminium (Al 99,99 % mass fraction), transfer into a 400 ml beaker and cover
with a watch glass. Dissolve it in 50 ml hydrochloric acid solution (4.2). After cooling, transfer the solution
quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well.
1 ml of this solution contains 1 mg of Al.
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CEN/TS 15605:2007 (E)
4.11 Antimony stock solution, 1 g/l Sb
Weigh (0,5 ± 0,001) g of pure antimony (Sb 99,99 % mass fraction), transfer into a 250 ml beaker and cover
with a watch glass. Dissolve it in 50 ml hydrochloric acid (4.1) and 25 ml of nitric acid solution (4.4). Heat gen-
tly until the metal is dissolved. After cooling, transfer the solution quantitatively into a 500 ml one-mark volu-
metric flask, containing 100 ml of hydrochloric acid (4.1), dilute to the mark with water and mix well.
1 ml of this solution contains 1 mg of Sb.
4.12 Arsenic stock solution, 1 g/l As
Weigh (0,5 ± 0,001) g of pure arsenic (As 99,99 % mass fraction), transfer into a 250 ml beaker and cover
with a watch glass. Dissolve it in 20 ml of nitric acid solution (4.4). Heat gently until the metal is dissolved.
After cooling, transfer the solution quantitatively into a 500 ml one-mark volumetric flask, dilute to the mark
with water and mix well.
1 ml of this solution contains 1 mg of As.
4.13 Beryllium stock solution, 5 g/l Be
Weigh (1 ± 0,001) g of pure beryllium (Be 99,99 % mass fraction), transfer into a 250 ml beaker and cover
with a watch glass. Dissolve it in 40 ml hydrochloric acid (4.1). Heat gently until the metal is dissolved. After
cooling, transfer the solution quantitatively into a 200 ml one-mark volumetric flask, dilute to the mark with
water and mix well.
1 ml of this solution contains 5 mg of Be.
4.14 Beryllium stock solution, 1 g/l Be
Weigh (0,5 ± 0,001) g of pure beryllium (Be 99,99 % mass fraction), transfer into a 250 ml beaker and cover
with a watch glass. Dissolve it in 20 ml hydrochloric acid (4.1). Heat gently until the metal is dissolved. After
cooling, transfer the solution quantitatively into a 500 ml one-mark volumetric flask, dilute to the mark with wa-
ter and mix well.
1 ml of this solution contains 1 mg of Be.
4.15 Cadmium stock solution, 1 g/l Cd
Weigh (1 ± 0,001) g of pure cadmium (Cd 99,99 % mass fraction), transfer into a 400 ml beaker and cover
with a watch glass. Dissolve it in 10 ml nitric acid (4.3). Heat gently until the metal is dissolved, then boil until
nitrous fumes have been expelled. After cooling, transfer the solution quantitatively into a 1 000 ml one-mark
volumetric flask, dilute to the mark with water and mix well.
1 ml of this solution contains 1 mg of Cd.
4.16 Cobalt stock solution, 5 g/l Co
Weigh (1 ± 0,001) g of pure cobalt (Co 99,99 % mass fraction), transfer into a 250 ml beaker and cover with a
watch glass. Dissolve it in 10 ml hydrochloric acid (4.1) and 10 ml of nitric acid (4.3). Heat gently until the
metal is dissolved, then boil until nitrous fumes have been expelled. After cooling, transfer the solution quanti-
tatively into a 200 ml one-mark volumetric flask, dilute to the mark with water and mix well.
1 ml of this solution contains 5 mg of Co.
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CEN/TS 15605:2007 (E)
4.17 Cobalt stock solution, 1 g/l Co
Weigh (0,5 ± 0,001) g of pure cobalt (Co 99,99 % mass fraction), transfer into a 250 ml beaker and cover with
a watch glass. Dissolve it in 5 ml hydrochloric acid (4.1) and 5 ml of nitric acid (4.3). Heat gently until the metal
is dissolved, then boil until nitrous fumes have been expelled. After cooling, transfer the solution quantitatively
into a 500 ml one-mark volumetric flask, dilute to the mark with water and mix well.
1 ml of this solution contains 1 mg of Co.
4.18 Iron stock solution, 5 g/l Fe
Weigh (5 ± 0,001) g of pure iron (Fe 99,99 % mass fraction), transfer into a 400 ml beaker and cover with a
watch glass. Dissolve it in 100 ml hydrochloric acid (4.1) and 50 ml of nitric acid solution (4.4). Heat gently
until the metal is dissolved, then boil until nitrous fumes have been expelled. After cooling, transfer the solu-
tion quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well.
1 ml of this solution contains 5 mg of Fe.
4.19 Iron stock solution, 1 g/l Fe
Weigh (1 ± 0,001) g of pure iron (Fe 99,99 % mass fraction), transfer into a 250 ml beaker and cover with a
watch glass. Dissolve it in 20 ml hydrochloric acid (4.1) and 10 ml of nitric acid solution (4.4). Heat gently until
the metal is dissolved, then boil until nitrous fumes have been expelled. After cooling, transfer the solution
quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well.
1 ml of this solution contains 1 mg of Fe.
4.20 Lead stock solution, 5 g/l Pb
Weigh (2,5 ± 0,001) g of pure lead (Pb 99,99 % mass fraction), transfer into a 400 ml beaker and cover with a
watch glass. Dissolve it in 50 ml of nitric acid solution (4.4). Heat gently until the metal is dissolved, then boil
until nitrous fumes have been expelled. After cooling, transfer the solution quantitatively into a 500 ml one-
mark volumetric flask, dilute to the mark with water and mix well.
1 ml of this solution contains 5 mg of Pb.
4.21 Lead stock solution, 1 g/l Pb
Weigh (1 ± 0,001) g of pure lead (Pb 99,99 % mass fraction), transfer into a 250 ml beaker and cover with a
watch glass. Dissolve it in 20 ml of nitric acid solution (4.4). Heat gently until the metal is dissolved, then boil
until nitrous fumes have been expelled. After cooling, transfer the solution quantitatively into a 1 000 ml one-
mark volumetric flask, dilute to the mark with water and mix well.
1 ml of this solution contains 1 mg of Pb.
4.22 Magnesium stock solution, 1 g/l Mg
Weigh (1 ± 0,001) g of pure magnesium (Mg 99,99 % mass fraction), transfer into a 250 ml beaker and cover
with a watch glass. Dissolve it in 50 ml of nitric acid solution (4.4). Heat gently until the metal is dissolved, then
boil until nitrous fumes have been expelled. After cooling, transfer the solution quantitatively into a 1 000 ml
one-mark volumetric flask, dilute to the mark with water and mix well.
1 ml of this solution contains 1 mg of Mg.
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CEN/TS 15605:2007 (E)
4.23 Manganese stock solution, 5 g/l Mn
The manganese 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 60 ml to 80 ml of sulphuric acid (4,5 mol/l) and approxi-
mately 100 ml of water. Shake and after a few seconds, allow the solution to settle and add water. Repeat the
water cleaning several times. Remove the metallic manganese, introduce it into acetone, allow to settle and
dry the metal in an oven at 100 °C for 2 min. Cool in a dessicator.
Weigh (5 ± 0,001) g of this purified manganese and transfer into a 400 ml beaker and cover with a watch
glass. Dissolve it in 50 ml hydrochloric acid (4.1) and 125 ml of nitric acid solution (4.4). Heat gently until the
metal is dissolved. After cooling, transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask,
dilute to the mark with water and mix well.
1 ml of this solution contains 5 mg of Mn.
4.24 Manganese stock solution, 1 g/l Mn
Weigh (1 ± 0,001) g of manganese, purified as described in 4.23, transfer into a 250 ml beaker and cover with
a watch glass. Dissolve it in 10 ml hydrochloric acid (4.1) and 25 ml of nitric acid solution (4.4). Heat gently
until the metal is dissolved. After cooling, transfer the solution quantitatively into a 1 000 ml one-mark volumet-
ric flask, dilute to the mark with water and mix well.
1 ml of this solution contains 1 mg of Mn.
4.25 Nickel stock solution, 10 g/l Ni
Weigh (5 ± 0,001) g of pure nickel (Ni 99,99 % mass fraction), transfer into a 400 ml beaker and cover with a
watch glass. Dissolve it in 125 ml of nitric acid solution (4.4). Heat gently until the metal is dissolved, then boil
until nitrous fumes have been expelled. After cooling, transfer the solution quantitatively into a 500 ml one-
mark volumetric flask, dilute to the mark with water and mix well.
1 ml of this solution contains 10 mg of Ni.
4.26 Nickel stock solution, 5 g/l Ni
Weigh (5 ± 0,001) g of pure nickel (Ni 99,99 % mass fraction), transfer into a 400 ml beaker and cover with a
watch glass. Dissolve it in 125 ml of nitric acid solution (4.4). Heat gently until the metal is dissolved, then boil
until nitrous fumes have been expelled. After cooling, transfer the solution quantitatively into a 1 000 ml one-
mark volumetric flask, dilute to the mark with water and mix well.
1 ml of this solution contains 5 mg of Ni.
4.27 Nickel stock solution, 1 g/l Ni
Weigh (1 ± 0,001) g of pure nickel (Ni 99,99 % mass fraction), transfer into a 250 ml beaker and cover with a
watch glass. Dissolve it in 25 ml of nitric acid solution (4.4). Heat gently until the metal is dissolved, then boil
until nitrous fumes have been expelled. After cooling, transfer the solution quantitatively into a 1 000 ml one-
mark volumetric flask, dilute to the mark with water and mix well.
1 ml of this solution contains 1 mg of Ni.
4.28 Phosphorus stock solution, 1 g/l P
Weigh (4,394 ± 0,001) g of dried potassium dihydrogenphosphate, transfer into a 250 ml beaker and dissolve
it with water. Transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark
with water and mix well.
1 ml of this solution contains 1 mg of P.
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CEN/TS 15605:2007 (E)
4.29 Tin stock solution, 10 g/l Sn
Weigh (5 ± 0,001) g of pure tin (Sn 99,99 % mass fraction), transfer into a 400 ml beaker and cover with a
watch glass. Dissolve it in 50 ml hydrochloric acid (4.1). Heat gently until the metal is dissolved. After cooling,
transfer the solution quantitatively into a 500 ml one-mark volumetric flask, dilute to the mark with water and
mix well.
1 ml of this solution contains 10 mg of Sn.
4.30 Tin stock solution, 5 g/l Sn
Weigh (2,5 ± 0,001) g of pure tin (Sn 99,99 % mass fraction), transfer into a 400 ml beaker and cover with a
watch glass. Dissolve it in 50 ml hydrochloric acid (4.1). Heat gently until the metal is dissolved. After cooling,
transfer the solution quantitatively into a 500 ml one-mark volumetric flask, dilute to the mark with water and
mix well.
1 ml of this solution contains 5 mg of Sn.
4.31 Tin stock solution, 1 g/l Sn
Weigh (0,5 ± 0,001) g of pure tin (Sn 99,99 % mass fraction), transfer into a 250 ml beaker and cover with a
watch glass. Dissolve it in 50 ml hydrochloric acid (4.1). Heat gently until the metal is dissolved. After cooling,
transfer the solution quantitatively into a 500 ml one-mark volumetric flask, dilute to the mark with water and
mix well.
1 ml of this solution contains 1 mg of Sn.
4.32 Zinc stock solution, 10 g/l Zn
Weigh (5 ± 0,001) g of pure zinc (Zn 99,99 % mass fraction), transfer into a 400 ml beaker and cover with a
watch glass. Dissolve it in 250 ml hydrochloric acid solution (4.2). Heat gently until the metal is dissolved. After
cooling, transfer the solution quantitatively into a 500 ml one-mark volumetric flask, dilute to the mark with wa-
ter and mix well.
1 ml of this solution contains 10 mg of Zn.
4.33 Zinc stock solution, 1 g/l Zn
Weigh (1 ± 0,001) g of pure zinc (Zn 99,99 % mass fraction), transfer into a 400 ml beaker and cover with a
watch glass. Dissolve it in 50 ml hydrochloric acid solution (4.2). Heat gently until the metal is dissolved. After
cooling, transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with
water and mix well.
1 ml of this solution contains 1 mg of Zn.
4.34 Internal standard solution, 1g/l Yttrium in 0,5 M nitric acid.
5 Apparatus
5.1 Ordinary laboratory apparatus.
5.2 Optical emission spectrometer (OES), equipped with inductively coupled plasma (ICP) and nebuli-
sation systems
The instrument used will be considered satisfactory if, after optimizing in accordance with the manufacturer’s
instructions, it meets the performance criteria given in Annex A.
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CEN/TS 15605:2007 (E)
6 Sampling
Sampling shall be carried out in accordance with ISO 1811-1 or ISO 1811-2 as appropriate.
Test samples shall be in the form of fine chips, drillings or millings e.g. with a maximum thickness of 0,5 mm.
7 Procedure
7.1 Method A: Coppers
7.1.1 Preparation of the test portion solution
7.1.1.1 Test portion
Weigh (1 ± 0,001) g of the test sample.
7.1.1.2 Test portion solution 5 g/l
Transfer the test portion (7.1.1.1) into a 250 ml beaker.
Add 20 ml of hydrochloric acid solution (4.2) and 5 ml of nitric acid (4.3). Cover and heat gently until the sam-
ple is completely dissolved, then heat to boiling. Allow to cool. Rinse the beaker cover and the walls of the
beaker with water.
Transfer the dissolved test portion into a 200 ml one-mark volumetric flask containing 10 ml of hydrochloric
acid (4.1). Dilute to the mark with water and mix well.
7.1.1.3 Test portion solution 1 g/l
In order to obtain solutions with 1 g/l concentration, pipette exactly 20 ml of test portion solution (7.1.1.2) into a
100 ml one-mark volumetric flask containing 5 ml of hydrochloric acid (4.1) and 5 ml of yttrium solution (4.33).
Dilute to the mark with water and mix well.
7.1.2 Check test
Make a preliminary check of the apparatus by preparing a solution of a copper reference material or a
synthetic sample containing known amounts of the elements listed in Table 1 and carrying out the procedure
specified in 7.1.4.
7.1.3 Establishment of the calibration curves
7.1.3.1 Preparation of the calibration solutions
7.1.3.1.1 General
In all cases the acidity of the calibration solutions shall be similar to that of the test portion solutions.
7.1.3.1.2 Preparation of the 5 g/l calibration solutions, using mono-elemental solutions
Weigh the quantities of copper (4.7) shown in Table 8 and introduce them into each of a series of 250 ml
beakers.
Add 20 ml of the hydrochloric acid solution (4.2) to each beaker.
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CEN/TS 15605:2007 (E)
With calibrated pipettes, add the volumes of the elemental solutions of Sn, Pb, Zn, Fe, Ni, Mn, P, Al, Be, Co
and Cd shown in Table 8 to each beaker and 5 ml of nitric acid (4.3).
Heat gently in order to dissolve copper and then rinse the walls of the beaker with water. Cover with a watch
glass and heat to boiling.
Allow to cool and transfer each calibration solution into a 200 ml one-mark volumetric flask containing 10 ml of
hydrochloric acid (4.1). Dilute to the mark with water and mix well.
7.1.3.1.3 Preparation of the 1 g/l calibration solutions
Dilute accurately the 5 g/l calibration solution (7.1.3.1.2) in order to obtain 1 g/l calibration solutions.
Pipette exactly 20 ml of the 5 g/l calibration solutions (7.1.3.1.2) into 100 ml one-mark volumetric flasks each
containing 5 ml of hydrochloric acid (4.1) and 5 ml of yttrium solution (4.34). Dilute to the mark with water and
mix well.
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CEN/TS 15605:2007 (E)
Table 8 — Method A — Composition of the 5 g/l calibration solutions
Label Drift survey
Element
solution
P1 P2 P3
(see 7.1.3.3)
Cu 976,3 mg 973,3 mg 979,4 mg 988,0 mg
(4.7) 97,63 % 97,33 % 97,94 % 98,80 %
Sn 0,2 mg 0,5mg 6,0 mg 1,0 mg
a b
(4.31) 6 ml 1 ml
0,02 % 0,05 % 0,60 % 0,10 %
Pb 6,0 mg 0,5mg 0,2mg 1,0 mg
(4.21) 6 ml c d 1 ml
0,60 % 0,05 % 0,02 % 0,10 %
Zn 0,2mg 0,5 mg 6,0 mg 1,0 mg
e f
(4.33) 6 ml 1 ml
0,02 % 0,05 % 0,60 % 0,10 %
Fe 0,5 mg 6,0 mg 0,1 mg 1,0 mg
g h
(4.19) 6 ml 1 ml
0,05 % 0,60 % 0,01 % 0,10 %
Ni 0,1 mg 6,0 mg 0,5 mg 1,0 mg
i j
(4.27) 6 ml 1 ml
0,01 % 0,60 % 0,05 % 0,10 %
Mn 6,0 mg 0,1 mg 0,5 mg 1,0 mg
(4.24) 6 ml k l 1 ml
0,60 % 0,01 % 0,05 % 0,10 %
P 4,0 mg 0,1 mg 0,5 mg 2,0 mg
m n
(4.28) 4 ml 2 ml
0,40 % 0,01 % 0,05 % 0,20 %
Al 6,0 mg 0,5 mg 0,2mg 1,0 mg
o p
(4.10) 6 ml 1 ml
0,60 % 0,05 % 0,02 % 0,10 %
Be 0,5 mg 6,0 mg 0,1 mg 1,0 mg
q r
(4.14) 6 ml 1 ml
0,05 % 0,60 % 0,01 % 0,10 %
Co 0,1 mg 6,0 mg 0,5 mg 1,0 mg
(4.17) s 6 ml t 1 ml
0,01 % 0,60 % 0,05 % 0,10 %
Cd 0,1 mg 0,5 mg 6,0 mg 1,0 mg
u v
(4.15) 6 ml 1 ml
0,01 % 0,05 % 0,60 % 0,10 %
a l
2 ml of a 0,1 g/l tin stock solution 5 ml of a 0,1 g/l manganese stock solution
b m
5 ml of a 0,1 g/l tin stock solution 1 ml of a 0,1 g/l phosphorus stock solution
c n
5 ml of a 0,1 g/l lead stock solution 5 ml of a 0,1 g/l phosphorus stock solution
d o
2 ml of a 0,1 g/l lead stock solution 5 ml of a 0,1 g/l aluminium solution
e p
2 ml of a 0,1 g/l zinc stock solution 2 ml of a 0,1 g/l aluminium stock solution
f q
5 ml of a 0,1 g/l zinc stock solution 5 ml of a 0,1 g/l beryllium stock solution
g r
5 ml of a 0,1 g/l iron stock solution 1 ml of a 0,1 g/l beryllium stock solution
h s
1 ml of a 0,1 g/l iron stock solution 1 ml of a 0,1 g/l cobalt stock solution
i t
1 ml of a 0,1 g/l nickel stock solution 5 ml of a 0,1 g/l cobalt stock solution
u
j
1 ml of a 0,1 g/l cadmium stock solution
5 ml of a 0,1 g/l nickel stock solution
k v
1 ml of a 0,1 g/l manganese stock solution 5 ml of a 0,1 g/l cadmium stock solution
14
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CEN/TS 15605:2007 (E)
7.1.3.2 Adjustment of the apparatus
Start the ICP-OES and let it run for at least half an hour before taking any measurements.
Adjust all the instrumental parameters, each gas (outer, intermediate or central) flow rate, torch position,
entrance slits, exit slits, photomultiplier tubes voltages, wavelengths of the analytical lines specified in Table 9,
pre-spraying time and integrating time, according to the manufacturer’s instructions, while aspirating (for each
element) the highest concentration calibration solution.
Prepare the software to measure the intensity, mean value and relative standard deviation of each analytical
line.
Each time the internal standard is used (Y line 371,03 nm), prepare the software to calculate the ratio between
each analyte intensity and internal standard intensity.
Table 9 — Wavelengths for determinations in coppers
Wavelength
Element
nm
Sn 189,90
Pb 220,30
a
Zn
334,55
Fe 238,20
Ni 231,60
Mn 257,60
Al 308,20
P 178,23
Be 313,00
Co 228,60
Cd 226,50
a
206,20 nm and 213,80 nm wavelengths may be used to determine zinc, pro-
vided that interference from copper has been investigated.
7.1.3.3 Spectrometric measurements of the calibration solutions
Carry out the spectrometric measurements of the 1 g/l solutions identified P1, P2, P3 (see Table 8 and
7.1.3.1.3). For phosphorus use the 5 g/l calibration solutions (7.1
...
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