SIST EN 13806-2:2025
(Main)Foodstuffs - Determination of trace elements - Part 2: Determination of total mercury in foodstuffs by atomic fluorescence spectrometry (AFS) - Cold vapour technique after pressure digestion
Foodstuffs - Determination of trace elements - Part 2: Determination of total mercury in foodstuffs by atomic fluorescence spectrometry (AFS) - Cold vapour technique after pressure digestion
This document specifies a method for the determination of total mercury in foodstuffs by cold vapour atomic fluorescence spectrometry (AFS) after pressure digestion.
This method was tested in a collaborative study carried out in connection with the pressure digestion method EN 13805 on seven different materials with a mercury concentration in the range from 0,006 mg/kg to 5,38 mg/kg and successfully validated in this range.
The following foodstuffs were analysed: Saithe (dried); Celery (dried); Wheat noodle powder; Wild mushrooms (dried); Pig liver (dried); Cacao powder; Tuna fish (dried).
The lower limit of the method’s applicabilitiy varies depending on the food matrix and the water content of the foodstuff. It is a laboratory-specific value and is defined by the laboratory when calculating the limit of quantification.
Lebensmittel - Bestimmung von Elementspuren - Teil 2: Bestimmung des Gesamtquecksilbers in Lebensmitteln mittels Atomfluoreszenzspektrometrie (AFS) - Kaltdampftechnik nach Druckaufschluss
Dieses Dokument legt ein Verfahren zur Bestimmung des Gesamtquecksilbers in Lebensmitteln mit Atomfluoreszenzspektrometrie-(AFS-)Kaltdampftechnik nach Druckaufschluss fest.
Dieses Verfahren wurde in einem Ringversuch geprüft, der in Verbindung mit dem Druckaufschlussverfahren aus EN 13805 an sieben verschiedenen Materialien mit einem Quecksilbergehalt im Bereich von 0,006 mg/kg bis 5,38 mg/kg durchgeführt wurde, und wurde für diesen Bereich erfolgreich validiert.
Die folgenden Lebensmittel wurden analysiert:
- Seelachs (getrocknet);
- Staudensellerie (getrocknet);
- Weizennudelpulver;
- Wildpilze (getrocknet);
- Schweineleber (getrocknet);
- Kakaopulver;
- Thunfisch (getrocknet).
Die untere Grenze der Anwendbarkeit des Verfahrens variiert in Abhängigkeit von der Lebensmittelmatrix und vom Wassergehalt des Lebensmittels. Sie ist laborspezifisch und wird bei der Ermittlung der Bestimmungsgrenze durch das Labor festgelegt (siehe 9.2).
Produits alimentaires - Dosage des éléments traces - Partie 2 : Dosage du mercure total dans les produits alimentaires par spectrométrie de fluorescence atomique (SFA) - Génération de vapeurs froides après digestion sous pression
Le présent document spécifie une méthode pour le dosage du mercure total dans les produits alimentaires par spectrométrie de fluorescence atomique (SFA) à vapeurs froides après digestion sous pression.
Cette méthode a été testée dans le cadre d’une étude interlaboratoires réalisée en lien avec l’EN 13805 relative à la méthode de la digestion sous pression, sur sept matériaux différents dans lesquels la concentration du mercure variait entre 0,006 mg/kg et 5,38 mg/kg, et a été validée pour ce domaine de concentration.
Les produits alimentaires suivants ont été analysés :
— Lieu noir (séché) ;
— Céleri (séché) ;
— Nouilles de blé en poudre ;
— Champignons sauvages (séchés) ;
— Foie de porc (séché) ;
— Cacao en poudre ;
— Thon (séché).
Le seuil d’applicabilité de la méthode varie en fonction de la matrice alimentaire et de la teneur en eau du produit alimentaire. Il s’agit d’une valeur spécifique au laboratoire, définie par celui-ci lors du calcul de la limite de quantification (voir 9.2).
Živila - Določevanje elementov v sledovih - 2. del: Določevanje celotnega živega srebra v živilih z atomsko fluorescenčno spektrometrijo (AFS) - Tehnika hladne pare po razklopu pod pritiskom
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-maj-2025
Nadomešča:
SIST EN 13806:2002
Živila - Določevanje elementov v sledovih - 2. del: Določevanje celotnega živega
srebra v živilih z atomsko fluorescenčno spektrometrijo (AFS) - Tehnika hladne
pare po razklopu pod pritiskom
Foodstuffs - Determination of trace elements - Part 2: Determination of total mercury in
foodstuffs by atomic fluorescence spectrometry (AFS) - Cold vapour technique after
pressure digestion
Lebensmittel - Bestimmung von Elementspuren - Teil 2: Bestimmung des
Gesamtquecksilbers in Lebensmitteln mittels Atomfluoreszenzspektrometrie (AFS) -
Kaltdampftechnik nach Druckaufschluss
Produits alimentaires - Dosage des éléments traces - Partie 2 : Dosage du mercure total
dans les produits alimentaires par spectrométrie de fluorescence atomique (SFA) -
Génération de vapeurs froides après digestion sous pression
Ta slovenski standard je istoveten z: EN 13806-2:2025
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.
EN 13806-2
EUROPEAN STANDARD
NORME EUROPÉENNE
March 2025
EUROPÄISCHE NORM
ICS 67.050 Supersedes EN 13806:2002
English Version
Foodstuffs - Determination of trace elements - Part 2:
Determination of total mercury in foodstuffs by atomic
fluorescence spectrometry (AFS) - cold vapour technique
after pressure digestion
Produits alimentaires - Dosage des éléments-traces - Lebensmittel - Bestimmung von Elementspuren - Teil
Partie 2 : Dosage du mercure total dans les produits 2: Bestimmung des Gesamtquecksilbers in
alimentaires par spectrométrie de fluorescence Lebensmitteln mittels Atomfluoreszenzspektrometrie
atomique (SFA) - Génération de vapeurs froides après (AFS) - Kaltdampftechnik nach Druckaufschluss
digestion sous pression
This European Standard was approved by CEN on 21 February 2025.
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-CENELEC 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-CENELEC Management
Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2025 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 13806-2:2025 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
Introduction . 4
1 Scope . 5
2 Normative references . 5
3 Terms and definitions . 5
4 Principle . 6
5 Reagents . 6
6 Apparatus . 9
7 Sampling . 10
8 Procedure. 10
8.1 Digestion, removal of nitrous gases and stabilization . 10
8.2 Cold vapour atomic fluorescence spectrometry . 11
8.2.1 Spectrometer settings . 11
8.2.2 Cold vapour AFS determination . 11
8.3 Quality control . 11
9 Evaluation . 11
9.1 Calculation . 11
9.2 Limit of quantification . 12
9.3 Precision . 13
9.4 Reproducibility . 13
9.5 Trueness . 13
10 Test report . 13
Annex A (informative) Precision data . 14
Bibliography . 16
European foreword
This document (EN 13806-2:2025) 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 September 2025, and conflicting national standards shall
be withdrawn at the latest by September 2025.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN 13806:2002.
The main changes compared to the previous edition are listed below:
— the document has been split up into three separate parts: EN 13806-1 covering the AAS-cold-vapour
technique, EN 13806-2 the AFS-cold-vapour technique and EN 13806-3 the solid sample AAS
technique;
— full technical revision to bring the technical realization up to date with the latest technology;
— Stabilization of the digest solution;
— Update of statistical data by new interlaboratory study.
Any feedback and questions on this document should be directed to the users’ national standards body.
A complete listing of these bodies can be found on the CEN website.
According to the CEN-CENELEC Internal Regulations, the national standards organisations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia,
Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland,
Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of North
Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and the United
Kingdom.
Introduction
This document has been developed in parallel with EN 13806-1 [3] and EN 13806-3 [4]. All three
methods were validated in parallel in interlaboratory studies with the same scope. They are statistically
compatible in performances. This allows the users of these documents to employ the most
appropriate/available method depending on the purpose of their studies. The statistical parameters of
these standards are presented in the respective documents.
1 Scope
This document specifies a method for the determination of total mercury in foodstuffs by cold vapour
atomic fluorescence spectrometry (AFS) after pressure digestion.
This method was tested in an interlaboratory study carried out in connection with the pressure digestion
method EN 13805 on seven different materials with a mercury concentration in the range from
0,006 mg/kg to 5,38 mg/kg and successfully validated in this range.
The following foodstuffs were analysed:
— Saithe (dried);
— Celery (dried);
— Wheat noodle powder;
— Wild mushrooms (dried);
— Pig liver (dried);
— Cacao powder;
— Tuna fish (dried).
The lower limit of the method’s applicability varies depending on the food matrix and the water content
of the foodstuff. It is a laboratory-specific value and is defined by the laboratory when calculating the
limit of quantification (see 9.2).
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements 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 elements and their chemical species - General considerations and
specific requirements
EN 13805, Foodstuffs - Determination of trace elements - Pressure digestion
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https://www.iso.org/obp
— IEC Electropedia: available at https://www.electropedia.org/
4 Principle
Mercury (Hg) is determined by AFS-cold-vapour technique in the test solution obtained by performing
the pressure digestion process specified in EN 13805.
The test solution is transferred into the reaction vessel of the mercury analyser to reduce the oxidized
forms of mercury to elemental mercury with bivalent tin or sodium borohydride. The elemental mercury
is then flushed into the cuvette of the AAS instrument using a carrier gas stream. The absorption at the
mercury line of 253,7 nm is used to determine the mercury concentration. In case of very small quantities
of mercury in the test solution, it is recommended to use a technique capable to concentrate the stripped
mercury on a gold/platinum gauze (amalgam technique) prior to determination.”
The total content of mercury is understood as the content measured using this specified method. It is
indicated in mg/kg or mg/l, depending on the samples type.
WARNING — The use of this method can involve the application of dangerous substances, actions or
equipment. Nevertheless, the method description cannot mention all dangers possibly involved in its
application. Each operator of the method is responsible for taking the appropriate safety precautions and
to respect the corresponding regulations.
5 Reagents
5.1 General
Unless otherwise specified, “solutions” are understood to be aqueous solutions.
The content of mercury in the chemicals and water shall be low enough not to affect the results.
5.2 Hydrochloric acid, ω = 30 % to 37 %, density = approx. 1,15 g/ml.
5.3 Nitric acid, ω = 65 % to 69 %, density = approx. 1,4 g/ml.
5.4 Diluted nitric acid
Nitric acid (5.3) + water, V + V , approx. 1 + 9.
1 2
5.5 Ascorbic acid solution, ϱ = 100 g/l.
Dissolve 10 g of ascorbic acid in 100 ml of water.
The solution remains stable for a maximum of one week.
5.6 Reducing agent
5.6.1 Tin(II) chloride solution, e.g. ϱ = 100 g/l.
Dissolve 50 g of tin(II) chloride, SnCI • 2 H 0, in approx. 100 ml of hydrochloric acid (5.2) in a 500 ml
2 2
volumetric flask and fill up to the mark with water. The solution shall be prepared freshly before use.
NOTE 1 The required concentration of tin(II) chloride depends on the analysis system and the concentration of
nitric acid in the measurement solution. Too low concentrations of tin(II) chloride could lead to insufficient
recoveries.
NOTE 2 Tin(II) chloride ages quickly, visible in light yellow precipitates of tin(IV) oxides. In case of higher
concentrations of tin(II) chloride, these precipitates occur more frequently.
NOTE 3 If necessary, the tin(II) chloride solution can be flushed with argon gas in order to remove any possible
traces of mercury.
5.7 Carrier solution
Diluted hydrochlor
...
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