Copper and copper alloys - Inductively coupled plasma optical emission spectrometry

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 Emissionsspektrometrie mit induktiv gekoppelter Plasmaanregung

Cuivre et alliages de cuivre - Analyse par spectrométrie d'émission optique avec source à 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

Status
Withdrawn
Publication Date
20-Nov-2007
Withdrawal Date
20-Jul-2010
Current Stage
9960 - Withdrawal effective - Withdrawal
Start Date
21-Jul-2010
Completion Date
21-Jul-2010

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SLOVENSKI STANDARD
01-januar-2008
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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
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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.

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

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.

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
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
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.
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).
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.
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.
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
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