CEN/TS 15023-3:2006
(Main)Copper and copper alloys - Determination of nickel content - Part 3: Flame atomic absorption spectrometry method (FAAS)
Copper and copper alloys - Determination of nickel content - Part 3: Flame atomic absorption spectrometry method (FAAS)
This Technical Specification specifies a flame atomic absorption spectrometric method (FAAS) for the determination of the nickel content of copper and copper alloys in the form of unwrought, wrought and cast products.
The method is applicable to products having a nickel mass fractions between 0,001 % and 6,0 %.
Kupfer und Kupferlegierungen - Bestimmung des Nickelgehaltes - Teil 3: Flammenatomabsorptionsspektrometrisches Verfahren (FAAS)
Diese Technische Spezifikation legt ein flammenatomabsorptionsspektrometrisches Verfahren (FAAS) für die Bestimmung des Nickelgehaltes in Kupfer und Kupferlegierungen fest, die als Gussstücke oder als plastisch oder nicht plastisch geformte Produkte vorliegen.
Das Verfahren ist geeignet für Produkte mit einem Nickel-Massenanteil zwischen 0,001 % und 6,0 %.
Cuivre et alliages de cuivre - Dosage du nickel - Partie 3: Méthode par spectrométrie d'absorption atomique dans la flamme (SAAF)
La présente Spécification Technique présente une méthode par spectrométrie d’absorption atomique dans la flamme (SAAF) pour le dosage du nickel dans le cuivre et les alliages de cuivre, sous forme de produits non corroyés, corroyés et moulés.
Cette méthode est applicable aux produits ayant des teneurs (fractions massiques) en nickel comprises entre 0,001 % et 6,0 %.
Baker in bakrove zlitine - Določevanje niklja - 3. del: Metoda s plamensko atomsko absorpcijsko spektrometrijo (FAAS)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-februar-2007
%DNHULQEDNURYH]OLWLQH'RORþHYDQMHQLNOMDGHO 0HWRGDVSODPHQVNRDWRPVNR
DEVRUSFLMVNRVSHNWURPHWULMR )$$6
Copper and copper alloys - Determination of nickel content - Part 3: Flame atomic
absorption spectrometry method (FAAS)
Kupfer und Kupferlegierungen - Bestimmung des Nickelgehaltes - Teil 3:
Flammenatomabsorptionsspektrometrisches Verfahren (FAAS)
Cuivre et alliages de cuivre - Dosage du nickel - Partie 3: Méthode par spectrométrie
d'absorption atomique dans la flamme (SAAF)
Ta slovenski standard je istoveten z: CEN/TS 15023-3:2006
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 15023-3
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
November 2006
ICS 77.120.30
English Version
Copper and copper alloys - Determination of nickel content -
Part 3: Flame atomic absorption spectrometry method (FAAS)
Cuivre et alliages de cuivre - Dosage du nickel - Partie 3: Kupfer und Kupferlegierungen - Bestimmung des
Méthode par spectrométrie d'absorption atomique dans la Nickelgehaltes - Teil 3:
flamme (SAAF) Flammenatomabsorptionsspektrometrisches Verfahren
(FAAS)
This Technical Specification (CEN/TS) was approved by CEN on 12 September 2006 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, 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
© 2006 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 15023-3:2006: E
worldwide for CEN national Members.
Contents Page
Foreword.3
1 Scope .4
2 Normative references .4
3 Principle.4
4 Reagents and materials .4
5 Apparatus .5
6 Sampling.6
7 Procedure .6
8 Expression of results .10
9 Precision.11
10 Test report .12
Bibliography .13
Foreword
This document (CEN/TS 15023-3:2006) has been prepared by Technical Committee CEN/TC 133 “Copper and
copper alloys”, the secretariat of which is held by DIN.
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 15023-3, Copper and copper alloys — Determination of nickel content — Part 3: Flame atomic absorption
spectrometry method (FAAS)
This is one of three parts of the standard/technical specification for the determination of nickel content in copper
and copper alloys. The other parts are:
prEN 15023-1, Copper and copper alloys — Determination of nickel content — Part 1: Spectrometric method
prEN 15023-2, Copper and copper alloys — Determination of nickel content — Part 2: Titrimetric method
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to announce this Technical Specification: Austria, Belgium, 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 the United
Kingdom.
1 Scope
This Technical Specification specifies a flame atomic absorption spectrometric method (FAAS) for the
determination of the nickel content of copper and copper alloys in the form of unwrought, wrought and cast
products.
The method is applicable to products having a nickel mass fractions between 0,001 % and 6,0 %.
2 Normative references
The following referenced documents are indispensable for the application of this European Technical Specification.
For dated references, 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
3 Principle
Dissolution of a test portion in hydrochloric and nitric acid solution followed, after suitable dilution and the addition
of lanthanum chloride to mask the effect of interfering ions, by aspiration into an air/acetylene flame of an atomic
absorption spectrometer. Measurement of the absorption of the 232,0 nm or the 352,4 nm line emitted by a nickel
hollow-cathode lamp.
4 Reagents and materials
4.1 General
During the analysis, use only reagents of recognized analytical grade and only distilled water or water of equivalent
purity.
4.2 Hydrochloric acid, HCl (ρ = 1,19 g/ml)
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) in 500 ml of water.
4.5 Lanthanum (III) chloride solution, 100 g/l
Dissolve 100 g of lanthanum (III) chloride (LaCl · 7H O) in a 600 ml beaker with water and transfer the solution into
3 2
a 1 000 ml one-mark volumetric flask. Dilute to the mark with water and mix.
4.6 Nickel stock solution, 1,0 g/l Ni
Weigh (1 ± 0,001) g of nickel (Ni ≥ 99,8 %) and transfer it into a 250 ml beaker. Dissolve it in 10 ml of hydrochloric
acid (4.2) and 10 ml of the nitric acid solution (4.4). Cover with a watch glass and, if necessary, heat gently to assist
dissolution. When 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 1,0 mg of Ni.
4.7 Nickel standard solution, 0,1 g/l Ni
Using a calibrated pipette, transfer 20,0 ml of nickel stock solution (4.6) into a 200 ml one-mark volumetric flask.
Dilute to the mark with water and mix.
Prepare this solution immediately prior to use.
1 ml of this solution contains 0,1 mg of Ni.
4.8 Nickel standard solution, 0,01 g/l Ni
Using a calibrated pipette, transfer 5,0 ml of nickel stock solution (4.6) into a 500 ml one-mark volumetric flask.
Dilute to the mark with water and mix.
Prepare this solution immediately prior to use.
1 ml of this solution contains 0,01 mg of Ni.
4.9 Copper base solution, 40 g/l Cu
Transfer 20,0 g of nickel-free copper (Cu ≥ 99,95 %) into an 800 ml beaker. Add 100 ml of hydrochloric acid (4.2)
and, cautiously, 200 ml of nitric acid solution (4.4). Cover with a watch glass and heat gently until the copper has
been completely dissolved, then heat up to the boiling point until the nitrous fumes have been expelled. Allow to
cool and transfer the solution quantitatively into a 500 ml one-mark volumetric flask, dilute to the mark with water
and mix.
4.10 Copper base solution, 2 g/l Cu
Transfer 25,0 ml of copper base solution (4.9) into a 500 ml one-mark volumetric flask. Add 95 ml of hydrochloric
acid (4.2) and 190 ml of nitric acid solution (4.4). Dilute to the mark with water and mix.
5 Apparatus
5.1 Ordinary laboratory apparatus
5.2 Burettes, 25 ml and 50 ml graduated in 0,05 ml or calibrated pipettes
5.3 Atomic absorption spectrometer, fitted with an air/acetylene burner
5.4 Nickel hollow-cathode lamp
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 drillings, chips or millings, with a maximum thickness of 0,3 mm.
7 Procedure
7.1 Preparation of the test portion solution
7.1.1 General
Prepare test portion solutions in accordance with 7.1.2, 7.1.3 or 7.1.4 depending on the expected nickel content of
the test sample.
7.1.2 Nickel mass fractions between 0,001 % and 0,012 %
Weigh (2 ± 0,001) g of the test sample.
Transfer the test portion into a 250 ml beaker. Add 10 ml of hydrochloric acid (4.2) and 20 ml of the nitric acid
solution (4.4). Cover with a watch glass and heat gently until the test portion is completely dissolved. Allow to cool.
Wash the beaker cover and the sides of the beaker with water.
Transfer the dissolved test portion quantitatively into a 100 ml one-mark volumetric flask. Add 10 ml of the
lanthanum (III) chloride solution (4.5). Dilute to the mark with water and mix.
7.1.3 Nickel mass fractions between 0,01 % and 0,25 %
Weigh (1 ± 0,001) g of the test sample.
Transfer the test portion into a 250 ml beaker. Add 5 ml of hydrochloric acid (4.2) and 10 ml of the nitric acid
solution (4.4). Cover with a watch glass and heat gently until the test portion is completely dissolved. Allow to cool.
Wash the beaker cover and the sides of the beaker with water.
Transfer the dissolved test portion quantitatively into a 100 ml one-mark volumetric flask. Add 10 ml of the
lanthanum (III) chloride solution (4.5). Dilute to the mark with water and mix.
7.1.4 Nickel mass fractions between 0,2 % and 6,0 %
Weigh (1 ± 0,001) g of the test sample.
Transfer the test portion into a 250 ml beaker. Add 5 ml of hydrochloric acid (4.2) and 10 ml of the nitric acid
solution (4.4). Cover with a watch glass and heat gently until the test portion is completely dissolved. Allow to cool.
Wash the beaker cover and the sides of the beaker with water.
Transfer the dissolved test portion quantitatively into a 100 ml one-mark volumetric flask. Dilute to the mark with
water and mix well. Transfer, by means of a calibrated pipette, 10,0 ml of this solution into a 200 ml one-mark
volumetric flask. Add 10 ml of hydrochloric acid (4.2), 20 ml of the nitric acid solution (4.4) and 20 ml of the
lanthanum (III) chloride solution (4.5). Dilute to the mark with water and mix.
7.2 Blank test
Carry out a blank test simultaneously with the determination, following the same procedure and using the same
quantities of all reagents as used for the determination, but omitting the test portion.
7.3 Check test
Make a preliminary check of the apparatus by preparing a solution of standard material or a synthetic sample
containing a known amount of nickel and of a composition similar to the material to be analysed. Carry out the
procedure specified in 7.5.
7.4 Establishment of the calibration curve
7.4.1 Preparation of the calibration solutions
7.4.1.1 General
In all cases, copper, chloride and nitrate concentrations, and acidity in the calibration solutions shall be similar to
those of the test portion solutions.
The presence of copper in the calibration solutions compensates for chemical interaction effects of copper in the
test portion solution. Normally no similar additions are required to compensate for the effect of alloying elements. If
any alloying element is present in the material to be analysed in mass fraction > 10 %, an appropriate mass of this
element shall be added to the calibration solutions.
The range of the calibration solutions is appropriate for most current models of equipment of average performance.
The range and operating conditions shall be selected for optimum measurements by the particular equipment
available, so that the curve of absorbance as a function of concentration is a straight line.
7.4.1.2 Nickel mass fractions between 0,001 % and 0,012 %
Into each of a series of seven 100 ml one-mark volumetric flasks, introduce the volumes of nickel standard solution
(4.8) using the burette or calibrated pipette (5.2) and copper base solution (4.9) shown in Table 1. Add 10 ml of
lanthanum (III) chloride solution (4.5). Dilute to the mark with water and mix.
Table 1 — Calibration for nickel mass fractions between 0,001 % and 0,012 5 %
Nickel Corresponding Corresponding Copper Corresponding Corresponding
standard nickel ni
...
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