SIST EN 15690-2:2009
(Main)Copper and copper alloys - Determination of iron content - Part 2: Flame atomic absorption spectrometric method (FAAS)
Copper and copper alloys - Determination of iron content - Part 2: Flame atomic absorption spectrometric method (FAAS)
This Part of this European Standard specifies a flame atomic absorption spectrometric method (FAAS) for the determination of the iron content of copper and copper alloys in the form of unwrought, wrought and cast products.
The method is applicable to products having iron mass fractions between 0,001 % and 5,0 %.
Kupfer und Kupferlegierungen - Bestimmung des Eisengehaltes - Teil 2: Flammenatomabsorptionsspektrometrisches Verfahren (FAAS)
Dieser Teil dieser Europäischen Norm legt ein flammenatomabsorptionsspektrometrisches Verfahren (FAAS)
für die Bestimmung des Eisengehaltes in Kupfer und Kupferlegierungen fest, die als Gussstücke oder als
plastisch oder nicht plastisch geformte Produkte vorliegen.
Das Verfahren ist geeignet für Produkte mit Eisengehalten zwischen 0,005 % und 5,0 % (Massenanteile).
Cuivre et alliages de cuivre - Dosage du fer - Partie 2 : Méthode par spectrométrie d'absorption atomique dans la flamme (SAAF)
La présente partie de cette Norme européenne spécifie une méthode de dosage par spectrométrie
d’absorption atomique dans la flamme (SAAF) du fer contenu dans le cuivre et les alliages de cuivre sous
forme de produits non corroyés, corroyés ou moulés.
La méthode est applicable aux produits ayant une teneur en fer comprise entre 0,005 % et 5,0 % (fraction
massique).
Baker in bakrove zlitine - Določevanje železa - 2. del: Metoda z uporabo spektrometrije s plamensko atomsko absorpcijo (FAAS)
General Information
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Kupfer und Kupferlegierungen - Bestimmung des Eisengehaltes - Teil 2: Flammenatomabsorptionsspektrometrisches Verfahren (FAAS)Cuivre et alliages de cuivre - Dosage du fer - Partie 2 : Méthode par spectrométrie d'absorption atomique dans la flamme (SAAF)Copper and copper alloys - Determination of iron content - Part 2: Flame atomic absorption spectrometric method (FAAS)77.120.30Baker in bakrove zlitineCopper and copper alloysICS:Ta slovenski standard je istoveten z:EN 15690-2:2009SIST EN 15690-2:2009en,fr01-april-2009SIST EN 15690-2:2009SLOVENSKI
STANDARD
SIST EN 15690-2:2009
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 15690-2February 2009ICS 77.040.30; 77.120.30 English VersionCopper and copper alloys - Determination of iron content - Part2: Flame atomic absorption spectrometric method (FAAS)Cuivre et alliages de cuivre - Dosage du fer - Partie 2 :Méthode par spectrométrie d'absorption atomique dans laflamme (SAAF)Kupfer und Kupferlegierungen - Bestimmung desEisengehaltes - Teil 2:Flammenatomabsorptionsspektrometrisches Verfahren(FAAS)This European Standard was approved by CEN on 26 December 2008.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the CEN 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 translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.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 STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2009 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15690-2:2009: ESIST EN 15690-2:2009
EN 15690-2:2009 (E) 2 Contents Page Foreword .3 1 Scope .4 2 Normative references .4 3 Principle .4 4 Reagents and materials .4 5 Apparatus .6 6 Sampling .6 7 Procedure .6 8 Expression of results . 10 9 Precision . 11 10 Test report . 12 Bibliography . 13
SIST EN 15690-2:2009
EN 15690-2:2009 (E) 3 Foreword This document (EN 15690-2:2009) has been prepared by Technical Committee CEN/TC 133 “Copper and copper alloys”, the secretariat of which is held by DIN. 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 August 2009, and conflicting national standards shall be withdrawn at the latest by August 2009. 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 standard: EN 15690-2, Copper and copper alloys — Determination of iron content — Part 2: Flame atomic absorption spectrometric method (FAAS) This is one of two Parts of the standard for the determination of iron content in copper and copper alloys. The other Part is: EN 15690-1, Copper and copper alloys — Determination of iron content — Part 1: Titrimetric method Part 1 will be the subject of future work. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: 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.
SIST EN 15690-2:2009
EN 15690-2:2009 (E) 4 1 Scope This Part of this European Standard specifies a flame atomic absorption spectrometric method (FAAS) for the determination of the iron content of copper and copper alloys in the form of castings or unwrought or wrought products. The method is applicable to products having iron mass fractions between 0,005 % and 5,0 %. 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 hydrochloric and nitric acid mixture followed, after suitable dilution and the addition of lanthanum chloride to mask the effect of interfering ions, by aspiration of the test solution into an air/acetylene flame of an atomic absorption spectrometer. Measurement of the absorption of the 248,3 nm or the 372,0 nm line emitted by an iron 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. Avoid any contamination with iron during the mechanical preparation steps.
4.2 Hydrochloric acid, HCl (ρ = 1,19 g/ml) 4.3 Nitric acid, HNO3 (ρ = 1,40 g/ml) 4.4 Nitric acid, (1 + 1) Add 500 ml of nitric acid (4.3) into 500 ml of water. 4.5 Hydrofluoric acid, HF (ρ = 1,13 g/ml) WARNING — Hydrofluoric acid is a hazardous substance. Care shall be taken and it shall be used under an efficient fume hood. SIST EN 15690-2:2009
EN 15690-2:2009 (E) 5 4.6 Lanthanum(III) chloride solution, 100 g/l Weigh 100 g of lanthanum(III) chloride (LaCl3 · 7H2O) in a 600 ml beaker, transfer it into a 1 000 ml one-mark volumetric flask and dissolve it with water. Dilute to the mark with water and mix well. 4.7 Iron stock solution, 0,5 g/l Fe a) Weigh (0,5 ± 0,001) g of high purity iron and transfer it into a 250 ml beaker. Dissolve it in 50 ml of hydrochloric acid (4.2), 25 ml water and 2,5 ml nitric acid (4.3). 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 well; or b) Weigh (0,715 ± 0,000 1) g of high purity iron(III) oxide (Fe2O3), previously dried and transfer it into a 250 ml beaker. Add 50 ml of hydrochloric acid (4.2). 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 well. 1 ml of this solution contains 0,5 mg of Fe. 4.8 Iron standard solution, 0,05 g/l Fe Transfer 20,0 ml of iron stock solution (4.7) into a 200 ml one-mark volumetric flask. Add 5 ml of hydrochloric acid (4.2), dilute to the mark with water and mix well. 1 ml of this solution contains 0,05 mg of Fe. 4.9 Iron standard solution, 0,01 g/l Fe Transfer 10,0 ml of iron stock solution (4.7) into a 500 ml one-mark volumetric flask. Add 10 ml of hydrochloric acid (4.2), dilute to the mark with water and mix well. 1 ml of this solution contains 0,01 mg of Fe. 4.10 Copper base solution, 20 g/l Cu Transfer (10 ± 0,01) g of iron-free copper (Cu ≥ 99,95 %) after etching into a 600 ml beaker. Add 100 ml of hydrochloric acid (4.2) and, cautiously, 100 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 well. 1 ml of this solution contains 0,02 g of Cu. 4.11 Copper base solution, 2,0 g/l Cu Transfer quantitatively 25 ml of copper base solution (4.10) into a 250 ml one-mark volumetric flask. Dilute to the mark with water and mix well. 1 ml of this solution contains 2,0 mg of Cu. SIST EN 15690-2:2009
EN 15690-2:2009 (E) 6 5 Apparatus 5.1 Atomic absorption spectrometer, fitted with an air/acetylene burner 5.2 Iron 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 beaker. Add 10 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. If undissolved matter remains, indicating the presence of silicon, filter the solution. Place the filter paper and contained salts in a platinum crucible and ash, taking care that the filter does not flame. Calcine at about 550 °C. Cool and add 5 ml of hydrofluoric acid (4.5) and five drops of nitric acid (4.3). Evaporate to dryness and calcine again for several minutes at about 700 °C to completely volatilize the silicon. Cool, and then dissolve the residue with the least possible volume of nitric acid solution (4.4). Filter, if necessary, and add this filtrate quantitatively to the original filtrate. 7.1.3 Iron mass fractions between 0,005 %
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