CEN/TS 15616:2009
(Main)Copper and copper alloys - Determination of cadmium content - Flame atomic absorption spectrometric method (FAAS)
Copper and copper alloys - Determination of cadmium content - Flame atomic absorption spectrometric method (FAAS)
This document specifies a flame atomic absorption spectrometric method (FAAS) for the determination of the cadmium content of copper and copper alloys in the form of castings or unwrought or wrought products.
The method is applicable to products having cadmium mass fractions between 0,002 % and 2,0 %.
Kupfer und Kupferlegierungen - Bestimmung des Cadmiumgehaltes - Flammenatomabsorptionsspektrometrisches Verfahren (FAAS)
Dieses Dokument legt ein flammenatomabsorptionsspektrometrisches Verfahren (FAAS) für die Bestimmung von Cadmiumgehalten in Kupfer und Kupferlegierungen fest, die als Gussstücke oder als plastisch oder nicht plastisch geformte Produkte vorliegen.
Das Verfahren ist geeignet für Produkte mit Cadmium-Massenanteilen zwischen 0,002 % und 2,0 %.
Cuivre et alliages de cuivre - Dosage du cadmium - Méthode par spectrométrie d'absorption atomique dans la flamme (SAAF)
Le présent document spécifie une méthode par spectrométrie d’absorption atomique dans la flamme (SAAF)
pour le dosage du cadmium dans le cuivre et les alliages de cuivre sous la forme de produits non corroyés,
corroyés ou moulés.
La méthode s’applique aux produits ayant des teneurs en cadmium comprises entre 0,002 % et 2,0 %.
Baker in bakrove zlitine - Določevanje kadmija - Metoda z uporabo spektrometrije s plamensko atomsko absorpcijo (FAAS)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-julij-2009
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SODPHQVNRDWRPVNRDEVRUSFLMR )$$6
Copper and copper alloys - Determination of cadmium content - Flame atomic absorption
spectrometry method (FAAS)
Kupfer und Kupferlegierungen - Bestimmung des Cadmiumgehaltes -
Flammenatomabsorptionsspektrometrisches Verfahren (FAAS)
Cuivre et alliages de cuivre - Dosage du cadmium - Méthode par spectrométrie
d'absorption atomique dans la flamme (SAAF)
Ta slovenski standard je istoveten z: CEN/TS 15616:2009
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 15616
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
April 2009
ICS 77.120.30
English Version
Copper and copper alloys - Determination of cadmium content -
Flame atomic absorption spectrometric method (FAAS)
Cuivre et alliages de cuivre - Dosage du cadmium - Kupfer und Kupferlegierungen - Bestimmung des
Méthode par spectrométrie d'absorption atomique dans la Cadmiumgehaltes -
flamme (SAAF) Flammenatomabsorptionsspektrometrisches Verfahren
(FAAS)
This Technical Specification (CEN/TS) was approved by CEN on 2 March 2009 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: Avenue Marnix 17, B-1000 Brussels
© 2009 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 15616:2009: 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 .5
7 Procedure .6
8 Expression of results . 10
9 Precision . 11
10 Test report . 11
Bibliography . 12
Foreword
This document (CEN/TS 15616:2009) 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.
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
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 document specifies a flame atomic absorption spectrometric method (FAAS) for the determination of the
cadmium content of copper and copper alloys in the form of castings or unwrought or wrought products.
The method is applicable to products having cadmium mass fractions between 0,002 % and 2,0 %.
2 Normative references
The following referenced documents are indispensable for the application 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.
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 standard, and cited at the appropriate
places in the text, are listed in the Bibliography.
3 Principle
Dissolution of a test portion in a fluoroboric-nitric acid mixture followed, after suitable dilution, by aspiration
into an air/acetylene flame of an atomic absorption spectrometer. Determination of the cadmium content by
measuring the absorption of the 228,8 nm line emitted by a cadmium hollow-cathode lamp.
4 Reagents and materials
During the analysis, use only reagents of recognized analytical grade and only distilled water or water of
equivalent purity.
4.1 Boric acid, H BO solution 40 g/l.
3 3
4.2 Hydrofluoric acid, HF 40 % (ρ = 1,13 g/ml).
4.3 Nitric acid, HNO (ρ = 1,40 g/ml).
4.4 Fluoroboric-nitric acid mixture
Mix together 300 ml of boric acid solution (4.1), 30 ml of hydrofluoric acid (4.2), 500 ml of nitric acid (4.3) and
150 ml of water.
4.5 Cadmium stock solution, 1,0 g/l Cd
Transfer (1 ± 0,001) g of cadmium (Cd ≥ 99,99 %) into a 250 ml tall-form beaker. Add 10 ml of water and 5 ml
of nitric acid (4.3), cover with a watch glass and heat gently (if necessary) until the cadmium is completely
dissolved. Boil gently to expel nitrous fumes. Allow to cool and transfer the solution quantitatively into a
1 000 ml one-mark volumetric flask. Add 100 ml of water and 20 ml of nitric acid (4.3). Dilute to the mark with
water and mix well.
1 ml of this solution contains 1 mg of Cd.
4.6 Cadmium standard solution, 0,050 g/l Cd
Transfer 10,0 ml of the cadmium stock solution (4.5) into a 200 ml one-mark volumetric flask. Add 100 ml of
water and 20 ml of nitric acid (4.3). Dilute to the mark with water and mix well. Prepare this solution
immediately prior to use.
1 ml of this solution contains 50,0 µg of Cd.
4.7 Cadmium standard solution, 0,005 g/l Cd
Transfer 20,0 ml of the cadmium standard solution (4.6) into a 200 ml one-mark volumetric flask. Add 100 ml
of water and 18 ml of nitric acid (4.3). Dilute to the mark with water and mix well. Prepare this solution
immediately prior to use.
1 ml of this solution contains 5,0 µg of Cd.
4.8 Copper base solution, 20 g/l Cu
Weigh 20,0 g of pure copper containing not more than 0,000 5 % Cd into a 1 000 ml beaker (5.1). Add 800 ml
of fluoroboric-nitric acid mixture (4.4). Heat gently until the copper is completely dissolved, then boil until
nitrous fumes have been expelled. In the case of polyethylene or polypropylene beakers, use a water bath for
heating. 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 well.
50 ml of this solution contain 1 g of Cu and 40 ml of solution (4.4).
5 Apparatus
5.1 Polytetrafluorethylene, polypropylene or low-pressure polyethylene beakers, capacity
250 ml and 1 000 ml.
5.2 Flasks, polytetrafluorethylene , polyethylene or polypropylene, capacities 250 ml and 600 ml.
5.3 Atomic absorption spectrometer, fitted with an air/acetylene burner.
5.4 Cadmium 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 0,5 mm.
7 Procedure
7.1 Preparation of the test portion solution
7.1.1 Test portion
Weigh (1 ± 0,001) g of the test sample.
7.1.2 Test portion solution
Transfer the test portion (7.1.1) into a 250 ml PTFE, polypropylene or low-pressure polyethylene beaker (5.1).
Add 40 ml of the attack reagent (4.4). Cover with a watch glass and heat gently until the test portion is
dissolved, then heat at a temperature of approximately 90 °C until nitrous fumes have been expelled. Wash
the cover and the sides of the beaker with water, and cool.
7.1.3 Cadmium mass fractions between 0,002 % and 0,075 %
Transfer the test portion solution (7.1.2) quantitatively into a 100 ml one-mark volumetric flask. Dilute to the
mark with water and mix well.
7.1.4 Cadmium mass fractions between 0,05 % and 0,75 %
Transfer the test portion solution (7.1.2) quantitatively into a 100 ml one-mark volumetric flask. Dilute to the
mark with water and mix well.
Transfer 10,0 ml of this solution into a 100 ml one-mark volumetric flask. Dilute to the mark with water and mix
well.
7.1.5 Cadmium mass fractions between 0,5 % and 2,0 %
Transfer the test portion solution (7.1.2) quantitatively into a 100 ml one-mark volumetric flask. Dilute to the
mark with water and mix well.
Transfer 20,0 ml of this solution into a 100 ml one-mark volumetric flask. Dilute to the mark with water and mix
well. Transfer 10 ml of this solution into a 100 ml one-mark volumetric flask. Dilute to the mark with water and
mix well.
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 substituting pure copper for the test portion
(7.1.1). Correct the result obtained from the determination in accordance with the result from the blank test.
7.3 Check test
Make a preliminary check of the apparatus by preparing a solution of a standard material or a synthetic
sample containing a known amount of cadmium and of composition similar to the material to be analysed.
Carry out the procedure specified in 7.5.
7.4 Establishment of the calibration solutions
7.4.1 Preparation of the calibration solutions
7.4.1.1 General
In all cases, copper, fluoride, borate and nitrate concentrations, and the pH-values of 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 solution. Normally no similar additions are required to compensate for the effect of alloying elements.
If an 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 volumes of copper base solution added (4.8)
have been calculated to compensate for chemical interaction effects of copper in test solutions of copper or
high-copper alloys. Overcompensation may occur if the same volumes are added when the test samples are
copper-based alloys where the percentage of copper is lower. In these cases the volumes of copper base
solution shall be decreased to match the copper content of the test sample in solution.
The cadmium concentration of the calibration solutions shall be adjusted to suit the sensitivity of the
spectrometer used, so that the curve of absorbance as a function of concentration is a straight line.
7.4.1.2 Cadmium mass fractions between 0,002 % and 0,075 %
Into each of a series of eight 100 ml one-mark volumetric flasks, introduce the volumes of cadmium standard
solutions (4.6 and 4.7) and of copper base solution (4.8) as shown in Table 1. Dilute to the mark with water
and mix well.
7.4.1.3 Cadmium mass fractions between 0,05 % and 0,75 %
Into each of a series of six 100 ml one-mark volumetric flasks, introduce the volumes of cadmium standard
solution (4.6) and of copper base solution (4.8) as shown in Table 2. Dilute to the mark with water and mix
well.
7.4.1.4 Cadmium mass fractions between 0,5 % and 2,0 %
Into each of a series of five 100 ml one-mark volumetric flasks, introduce the volumes of cadmium standard
solution (4.6) and of copper base solution (4.8) as shown in Table 3. Dilute to the mark with water and mix
well.
Table 1 — Calibration for cadmium mass fractions between 0,002 % and 0,075 %
Cadmium standard Corresponding Correspond
...
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