SIST EN 14546:2005

SLOVENSKI STANDARD
01-september-2005
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Foodstuffs - Determination of trace elements - Determination of total arsenic by hydride
generation atomic absorption spectrometry (HGAAS) after dry ashing
Lebensmittel - Bestimmung von Elementspuren - Bestimmung von Gesamtarsen mit
Atomabsorptionsspektrometrie-Hydridtechnik (HGAAS) nach Trockenveraschung
Produits alimentaires - Détermination des éléments traces - Détermination de l'arsenic
total par spectrométrie d'absorption atomique par génération d'hydrures (SAAGH) apres
calcination par voie seche
Ta slovenski standard je istoveten z: EN 14546:2005
ICS:
67.050 Splošne preskusne in General methods of tests and
analizne metode za živilske analysis for food products
proizvode
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EUROPEAN STANDARD
EN 14546
NORME EUROPÉENNE
EUROPÄISCHE NORM
April 2005
ICS 67.050
English version
Foodstuffs - Determination of trace elements - Determination of
total arsenic by hydride generation atomic absorption
spectrometry (HGAAS) after dry ashing
Produits alimentaires - Détermination des éléments traces - Lebensmittel - Bestimmung von Elementspuren -
Détermination de l'arsenic total par spectrométrie Bestimmung von Gesamtarsen mit
d'absorption atomique par génération d'hydrures (SAAGH) Atomabsorptionsspektrometrie-Hydridtechnik (HGAAS)
après calcination par voie sèche nach Trockenveraschung
This European Standard was approved by CEN on 15 March 2005.
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 Central Secretariat 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 Central Secretariat has the same status as the official
versions.
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, Slovakia,
Slovenia, Spain, Sweden, Switzerland and United Kingdom.
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EUROPÄISCHES KOMITEE FÜR NORMUNG
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© 2005 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 14546:2005: E
worldwide for CEN national Members.

Contents page
Foreword .3
1 Scope .4
2 Normative references .4
3 Principle.4
4 Reagents.4
5 Apparatus and equipment.6
6 Procedure .6
7 Calculation.8
8 Precision.8
9 Test report .9
Annex A (informative) Results of the inter-laboratory test.10
Bibliography.12

Foreword
This document (EN 14546:2005) 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 October 2005, and conflicting national standards shall be withdrawn at
the latest by October 2005.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic,
Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland
and United Kingdom.
1 Scope
This European Standard specifies a method for the determination of total arsenic in foodstuffs by hydride
generation atomic absorption spectrometry (HGAAS) after dry ashing.
Specific foodstuffs for which European Standards exist are excluded from the scope of this horizontal
European Standard. It is the task of the analyst to review if vertical standards exist.
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 13804, Foodstuffs – Determination of trace elements – Performance criteria, general considerations and
sample preparation.
3 Principle
The samples treated with nitric acid and ashing aid are evaporated to dryness and then mineralized at 425 °C
with a gradual increase in temperature. The ash is dissolved in hydrochloric acid and arsenic is quantified by
HGAAS-procedure at the arsenic line at 193,7 nm [1].
WARNING — The use of this standard may involve hazardous materials, operations and equipment.
This standard does not purport to address all the safety problems associated with its use. It is the
responsibility of the user of this standard to establish appropriate health and safety practices and
determine the applicability of regulatory limitations prior to use.
4 Reagents
4.1 General
The concentration of arsenic in the reagents and water used shall be low enough not to affect results of the
determination.
4.2 Hydrochloric acid
4.2.1 Hydrochloric acid, not less than 30 % of approximately ρ (HCl) = 1,15 g/ml.
4.2.2 Diluted hydrochloric acid, c ( ≈ 6 mol/l).
Dilute 500 ml hydrochloric acid (4.2.1) with water in a proportion of 1+1 parts by volume.
4.3 Nitric acid, not less than 65 % (mass fraction) of approximately p (HNO ) =1,4 g/ml.
1)
4.3.1 Diluted nitric acid 1, w = 32 %
To be prepared by mixing mix nitric acid (4.3) and water in a proportion of 1 + 1 parts by volume.
1)
4.3.2 Diluted nitric acid 2, w = 6,5 %
Mix nitric acid (4.3) and water in a proportion of 1 + 9 parts by volume.
1)
4.3.3 Diluted nitric acid 3, w = 3,3 %
Mix nitric acid (4.3) and water in a proportion of 1 + 19 parts by volume.
1)
4.4 Magnesium oxide, w = not less than 90 %
1)
4.5 Magnesium nitrate hexahydrate, w = not less than 98 %
4.6 Ashing aid
Suspend 20 g of magnesium nitrate hexahydrate (4.5) and 2 g of magnesium oxide (4.4) in 100 ml of water.
1)
4.7 Sodium hydroxide, w = not less than 95 %
1)
4.8 Potassium iodide, w = not less than 99,5 %
1)
4.9 Ascorbic acid, w =not less than 99,7 %
4.10 Pre-reducing solution
Dissolve 5 g of potassium iodide (4.8) and 5 g of ascorbic acid (4.9) in 100 ml of water.
4.11 Arsenic stock solution, in nitric acid, with a mass concentration ρ(As (V))=1 000 mg/l
The use of a stock solution accompanied by a certificate is advisable.
4.12 Arsenic calibration solutions
4.12.1 Intermediate standard solution
Prepare a standard of 25 µg/l in HCl (4.2.2) from the stock solution (4.11)
4.12.2 Calibration standards
Take an aliquot of the intermediate standard (e.g. 3 ml for a final concentration of 3 µg/l) and make up to 5 ml
with HCl (4.2.2). Add 5 ml of pre-reducing solution (4.10). Wait 30 min and make up to 25 ml with HCl (4.2.2).
Following the same procedure prepare at least three calibration standards at different concentrations plus the
zero point of the curve. The concentrations selected shall not exceed the linear range of the calibration curve
of arsenic.
1) w is the mass fraction.
1)
4.13 Sodium borohydride, w = not less than 96%
1)
4.14 Sodium hydroxide, w = not less than 98%
4.15 Sodium borohydride solution
The concentration of this reducing solution may vary according to the system of hydride generation employed
and the recommendations given by the manufacturer in the ma
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