SIST EN 15764:2010
(Main)Foodstuffs - Determination of trace elements - Determination of tin by flame and graphite furnace atomic absorption spectrometry (FAAS and GFAAS) after pressure digestion
Foodstuffs - Determination of trace elements - Determination of tin by flame and graphite furnace atomic absorption spectrometry (FAAS and GFAAS) after pressure digestion
This European Standard specifies a method for the determination of tin in foodstuffs and canned foods by flame and graphite furnace atomic absorption spectrometry (AAS) after pressurized digestion. The collaborative study included foodstuffs such as carrot puree, tomato puree, pineapple, mixed fruit, white wine, peach powder, tomato powder, powdered beans, powdered fruit yoghurt, fish powder, having mass fractions of tin ranging from 43 mg/kg to 260 mg/kg (Flame-AAS) and from 2,5 mg/kg to 269 mg/kg (Graphite Furnace AAS).
Lebensmittel - Bestimmung von Elementspuren - Bestimmung von Zinn mit Flammen- und Graphitofen- Atomabsorptionsspektrometrie (FAAS und GFAAS) nach Druckaufschluss
Dieses Dokument legt ein Verfahren zur quantitativen Bestimmung von Zinn in Lebensmitteln und Lebensmittelkonserven
durch Flammen- und Graphitofen-Atomabsorptionsspektrometrie (AAS) nach Druckaufschluss
fest. Im Ringversuch wurden Lebensmittel mit einem Zinngehalt von 43 mg/kg bis 260 mg/kg
(Flammen-AAS) und von 2,5 mg/kg bis 269 mg/kg (Graphitofen-AAS) untersucht.
Produits alimentaires - Dosage de l'étain par spectrométrie d'absorption atomique flamme (SAA) et spectrométrie d'absorption atomique à four graphite (GFAAS) après digestion sous pression
Le présent projet de norme spécifie un processus permettant de quantifier la teneur en étain des produits alimentaires et des conserves par spectrométrie d’absorption atomique flamme et spectrométrie d’absorption atomique à four graphite (AAS) après digestion sous pression.
Živila - Določevanje elementov v sledovih - Določevanje kositra s plamensko absorpcijsko spektroskopijo (FAAS) in atomsko absorpcijsko spektrometrijo z grafitno kiveto (GFAAS) po razklopu pod pritiskom
Ta evropski standard določa metodo za določanje kositra v živilih in konzervirani hrani s plamensko absorpcijsko spektrografijo z grafitno kiveto (AAS) po razklopu pod pritiskom. Sodelovalna študija vključuje živila kot na primer korenčkov pire, paradižnikov pire, ananas, mešano sadje, belo vino, breskve v prahu, paradižnik v prahu, fižol v prahu, sadni jogurt v prahu, ribe v prahu, ki imajo masne deleže kositra v razponu od 43 mg/kg do 260 mg/kg (plamen-AAS) in od 2,5 mg/kg do 269 mg/kg (grafitna kiveta AAS).
General Information
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Lebensmittel - Bestimmung von Elementspuren - Bestimmung von Zinn mit Flammen- und Graphitofen- Atomabsorptionsspektrometrie (FAAS und GFAAS) nach DruckaufschlussProduits alimentaires - Dosage de l'étain par spectrométrie d'absorption atomique flamme (SAA) et spectrométrie d'absorption atomique à four graphite (GFAAS) après digestion sous pressionFoodstuffs - Determination of trace elements - Determination of tin by flame and graphite furnace atomic absorption spectrometry (FAAS and GFAAS) after pressure digestion67.050Splošne preskusne in analizne metode za živilske proizvodeGeneral methods of tests and analysis for food productsICS:Ta slovenski standard je istoveten z:EN 15764:2009SIST EN 15764:2010en,fr,de01-marec-2010SIST EN 15764:2010SLOVENSKI
STANDARD
SIST EN 15764:2010
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 15764
December 2009 ICS 67.050 English Version
Foodstuffs - Determination of trace elements - Determination of tin by flame and graphite furnace atomic absorption spectrometry (FAAS and GFAAS) after pressure digestion
Produits alimentaires - Dosage des éléments traces - Dosage de l'étain par spectrométrie d'absorption atomique flamme (SAAF) et spectrométrie d'absorption atomique à four graphite (SAAFG) après digestion sous pression
Lebensmittel - Bestimmung von Elementspuren - Bestimmung von Zinn mit der Flammen- und Graphitofen-Atomabsorptionsspektrometrie (FAAS und GFAAS) nach Druckaufschluss This European Standard was approved by CEN on 7 November 2009.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards 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 translation under the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as the official 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 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 worldwide for CEN national Members. Ref. No. EN 15764:2009: ESIST EN 15764:2010
EN 15764:2009 (E) 2 Contents Page Foreword .31Scope .42Normative references .43Principle .44Reagents .45Apparatus and equipment .66Procedure .77Evaluations .98Precision . 109Test report . 11Annex A (informative)
Results of the inter-laboratory test . 12Bibliography . 16 SIST EN 15764:2010
EN 15764:2009 (E) 3 Foreword This document (EN 15764:2009) has been prepared by Technical Committee CEN/TC 275 “Food analysis - Horizontal methods”, 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 June 2010, and conflicting national standards shall be withdrawn at the latest by June 2010. 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 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 15764:2010
EN 15764:2009 (E) 4
1 Scope This European Standard specifies a method for the determination of tin in foodstuffs and canned foods by flame and graphite furnace atomic absorption spectrometry (AAS) after pressurized digestion.
The collaborative study included foodstuffs such as carrot puree, tomato puree, pineapple, mixed fruit, white wine, peach powder, tomato powder, powdered beans, powdered fruit yoghurt, fish powder, having mass fractions of tin ranging from 43 mg/kg to 260 mg/kg (Flame-AAS) and from 2,5 mg/kg to 269 mg/kg (Graphite Furnace AAS). 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. EN 13805, Foodstuffs — Determination of trace elements — Pressure digestion 3 Principle The sample is mineralized through pressurized digestion with nitric acid and hydrochloric acid in accordance with EN 13805. In the resulting digestion solution, tin is quantified by flame AAS (F-AAS) or graphite furnace AAS (GF-AAS) depending on the concentration in the sample solution. 4 Reagents 4.1 General The concentration of tin in the reagents and water used shall be low enough not to affect the results of the determination. 4.2 Nitric acid
Mass fraction w(HNO3) ≥ 65 %, mass concentration ρ(HNO3) ≈ 1,4 g/ml. 4.3 Hydrochloric acid
w(HCL) ≥ 30 %, ρ(HCl) ≈ 1,15 g/ml. 4.4 Tin stock solution
ρ(Sn) = 1 000 mg/l. 4.5 Tin standard and calibration solutions 4.5.1 General The standard and calibration solutions are prepared from the stock solution by dilution in glass volumetric flasks. For calibration, prepare at least four calibration solutions of different concentrations. The acid concen-tration shall correspond to the concentration in the measurement solution. SIST EN 15764:2010
EN 15764:2009 (E) 5 The preparation of the solutions in 4.5.2 and 4.5.3 is given as an example. 4.5.2 Calibration solutions
of ρ(Sn) = 5 mg/l, 10 mg/l, 20 mg/l and 30 mg/l for flame AAS. Fill four 50 ml volumetric flasks with 10 ml to 20 ml of water, add 5 ml of nitric acid (4.2) and 1 ml of hydrochloric acid (4.3) and mix. Cool the solutions to ambient temperature, and pipette exactly 0,25 ml, 0,50 ml, 1,00 ml and 1,50 ml of tin stock solution (4.4) for the respective calibration solutions of mass concentrations 5 mg/l, 10 mg/l, 20 mg/l and 30 mg/l into the four different 50 ml volumetric flasks. Mix the solutions and dilute to volume with water. These solutions are stable for at least one day. The calibration solutions described here shall be understood as examples. The concentrations prepared shall be in the linear range of the measuring device. The acid concentration of the calibration solutions shall be matched to the acid concentration in the sample solution. 4.5.3 Calibration solutions
of ρ(Sn) = 0,010 mg/l, 0,020 mg/l, 0,040 mg/l and 0,060 mg/l for GF-AAS. To prepare standard solution 1 (ρ(Sn) = 50 mg/l), fill a 50 ml volumetric flask with 10 ml to 20 ml of water, add 2,5 ml of hydrochloric acid (4.3) and mix. Cool the solution to ambient temperature, add exactly 2,5 ml of tin stock solution (4.4) and dilute to volume. This solution is stable for at least one week. To prepare standard solution 2 (ρ(Sn) = 1,0 mg/l), fill a 50 ml volumetric flask with 10 ml to 20 ml of water, add 2,5 ml of hydrochloric acid (4.3) and mix. Cool the solution to ambient temperature, add exactly 1,0 ml of tin standard solution 1 by pipette and dilute to volume.
Prepare the calibration solutions for the graphite furnace AAS from standard solution 2 according to the following procedure: Fill four 50 ml volumetric flasks with 10 ml to 20 ml of water, add 5 ml of nitric acid (4.2) and 1 ml of hydro-chloric acid (4.3) and mix. Cool the solutions to ambient temperature, pipette exactly 0,50 ml, 1,0 ml, 2,0 ml and 3,0 ml of standard solution 2 for the respective calibration solutions of mass concentrations 0,010 mg/l, 0,020 mg/l, 0,040 mg/l and 0,060 mg/l into the four different 50 ml volumetric flasks and dilute to final volume with water. These solutions shall be re-prepared for each day of measurement. The calibration solutions described here shall be understood as an example. The concentrations prepared shall be in the linear range of the measuring device. The acid concentration of the calibration solutions shall be matched to the amounts of acid used in the digestion. 4.6 Blank solution The blank solution contains water, nitric acid and hydrochloric acid in amounts that correspond to the concentrations in the measurement solution, for example 10 ml of nitric acid (4.2) and 2 ml of hydrochloric acid (4.3) in 100 ml of water. 4.7 Matrix modifiers for graphite furnace AAS 4.7.1 General Tin compounds shall be stabilized by matrix modifiers for quantification by graphite furnace AAS during the ashing step. Different matrix modifiers are used at different concentrations. To use a suitable modifier, first consider the recommendations of the device manufacturer. Select a suitable modifier; use the sample matrix to be examined to verify the ashing temperature of the graphite furnace program and optimize it in such a way that no tin is lost in the graphite tube during the mineralization step. SIST EN 15764:2010
EN 15764:2009 (E) 6 In 4.7.2 to 4.7.4 an example is presented of a modifier for quantifying tin. 4.7.2 Ammonium dihydrogen phosphate solution
Mass fraction w ≈ 10 %.
Dissolve 10,0 g of ammonium dihydrogen phosphate (NH4H2PO4) in 100 ml of water. 4.7.3 Magnesium nitrate solution
Mass concentration ρ(Mg) = 10 g/l. Dissolve 10,5 g of magnesium nitrate hexahydrate (Mg(NO3)2 ⋅ 6H2O) in 100 ml of water. NOTE Commercially available solutions can also be used. 4.7.4 Matrix modifiers for quantification of tin ρ(NH4H2PO4) = 50 µg/10 µl and ρ(Mg(NO3)2) = 3 µg/10 µl. Pipette 2,5 ml of ammonium dihydrogen phosphate solution (4.7.2) and 0,25 ml of magnesium nitrate solution (4.7.3) into a 50 ml volumetric flask; add 1 ml of nitric acid (4.2), and dilute to volume with water. This solution remains usable for several months when refrigerated. 5 Apparatus and equipment 5.1 General All apparatus and equipment that come into direct contact with the sample and solutions shall be pre-cleaned appropriately. 5.2 Atomic absorption spectrometer
with nitrous oxide/acetylene burner and atomization system. 5.3 Atomic absorption spectrometer
with background correction (Zeemann background correction is recommended), graphite tube furnace and autosampler. 5.4 Element-selective detection 5.4.1 Element-specific lamp
for tin (hollow-cathode or electrodeless discharge lamp). 5.4.2 Continuum radiation source
with high-resolution monochromatic illuminator as an alternative to 5.4.1. The resolution of the measuring equipment at normal operation shall correspond to at least the half-width value of the emission line of the element specific lamp (usually 1 pm to 3 pm). SIST EN 15764:2010
EN 15764:2009 (E) 7 6 Procedure 6.1 Digestion of the sample Mineralize the sample in pressurized digestion in accordance with EN 13805. For the quantification of tin, add 0,5 ml to 1 ml of hydrochloric acid (4.3) to the digestion vessel, which contains nitric acid (4.2) used for the digestion, at an amount that corresponds to the amount of nitric acid. Do not add the hydrochloric acid until the spontaneous reaction with nitric acid has subsided. After addition of the hydrochloric acid close the digestion vessel immediately in order to avoid loss of active chlorine. Start pressurized digestion shortly thereafter. The digestion requirements are based on the specifications of the instrument manufacturer, the reactivity of the sample, the maximum pressure stability of the digestion vessel and the attainable temperature. EXAMPLE Precisely weigh 0,4 g to 0,5 g of dry sample (residual moisture of less than 20 %) in a 100 ml digestion vessel and mix it with 5 ml of nitric acid (4.2). Carefully shake the digestion vessel to prevent clots from forming in the sample. After the spontaneous reaction has subsided, add 1 ml of hydrochloric acid (4.3) and close the digestion vessel as quickly as possible.
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