prEN 13806-3
(Main)Foodstuffs - Determination of trace elements - Part 3: Determination of total mercury in foodstuffs with atomic absorption directly from the foodstuff (elemental mercury analysis)
Foodstuffs - Determination of trace elements - Part 3: Determination of total mercury in foodstuffs with atomic absorption directly from the foodstuff (elemental mercury analysis)
This document specifies a method for the determination of total mercury (Hg) in foodstuffs using direct atomic absorption spectrometry after thermal decomposition in an oxygen or air flow and concentration by amalgam formation. The method is applicable for solid and liquid samples.
This method was tested in a collaborative study carried out on seven different materials with a mercury concentration in the range from 0,005 mg/kg to 5,20 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.
Lebensmittel - Bestimmung von Elementspuren - Teil 3: Bestimmung des Gesamtquecksilbers in Lebensmitteln durch Atomabsorption direkt aus dem Lebensmittel (Elementare Quecksilberanalyse)
Produits alimentaires - Dosage des éléments traces - Partie 3 : Dosage du mercure total dans les produits alimentaires par absorption atomique directe (analyse du mercure élémentaire)
Le présent document spécifie une méthode pour le dosage du mercure total (Hg) dans les produits alimentaires à l’aide de la spectrométrie d’absorption atomique directe, après décomposition thermique dans un flux d’oxygène ou d’air et concentration par amalgamation. La méthode est applicable aux échantillons solides et liquides.
Cette méthode a été testée dans le cadre d’une étude interlaboratoires réalisée sur sept matériaux différents dans lesquels la concentration du mercure variait entre 0,005 mg/kg et 5,20 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 - 3. del: Določevanje celotnega živega srebra v živilih z atomsko absorpcijo neposredno iz živila (elementarna analiza živega srebra)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-september-2023
Živila - Določevanje elementov v sledovih - 3. del: Določevanje celotnega živega
srebra v živilih z atomsko absorpcijo neposredno iz živila (elementarna analiza
živega srebra)
Foodstuffs - Determination of trace elements - Part 3: Determination of total mercury in
foodstuffs with atomic absorption directly from the foodstuff (elemental mercury analysis)
Lebensmittel - Bestimmung von Elementspuren - Teil 3: Bestimmung des
Gesamtquecksilbers in Lebensmitteln durch Atomabsorption direkt aus dem
Lebensmittel (Elementare Quecksilberanalyse)
Produits alimentaires - Dosage des éléments traces - Partie 3 : Dosage du mercure total
dans les produits alimentaires par absorption atomique directe (analyse du mercure
élémentaire)
Ta slovenski standard je istoveten z: prEN 13806-3
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.
DRAFT
EUROPEAN STANDARD
NORME EUROPÉENNE
EUROPÄISCHE NORM
June 2023
ICS 67.050 Will supersede EN 13806:2002
English Version
Foodstuffs - Determination of trace elements - Part 3:
Determination of total mercury in foodstuffs with atomic
absorption directly from the foodstuff (elemental mercury
analysis)
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee
CEN/TC 275.
If this draft becomes a European Standard, 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.
This draft European Standard was established by CEN 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.
Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are
aware and to provide supporting documentation.
Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without
notice and shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2023 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 13806-3:2023 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 . 8
7 Sampling . 8
8 Procedure . 8
8.1 Preparations for measurement . 8
8.1.1 Sample carrier cleaning . 8
8.1.2 Sample weight . 9
8.2 Direct atomic absorption spectrometry using thermal decomposition . 9
8.2.1 General. 9
8.2.2 Instrument blank value . 9
8.2.3 Instrument calibration and calibration control . 10
8.2.4 Measurement . 12
8.3 Quality control . 13
9 Evaluation . 13
9.1 Calculation . 13
9.2 Limit of quantification . 13
9.3 Precision . 14
9.4 Reproducibility . 14
9.5 Trueness . 14
10 Test report . 15
Annex A (informative) Explanations and notes . 16
Annex B (normative) Explanations and notes . 18
B.1 Use of sample carriers made of nickel . 18
B.2 Sample weight for different sample types . 18
B.3 Memory effects in the instrument system . 18
B.4 Exchange of catalyst and amalgamator units . 19
Bibliography . 20
European foreword
This document (prEN 13806-3:2023) has been prepared by Technical Committee CEN/TC 275 “Food
analysis – Horizontal methods”, the secretariat of which is held by DIN.
This document is currently submitted to the CEN Enquiry.
This document will supersede 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 collaborative study;
— full editorial revision.
This document was developed by the “Element Analysis” working group of the Federal Office of
Consumer Protection and Food Safety (BVL) according to the German Food and Feed Act, Paragraph 64.
Under preparation. Stage at the time of publication: prEN 13806-1:2023.
Under preparation. Stage at the time of publication: prEN 13806-2:2023.
Introduction
1 2
This document has been developed in parallel with EN 13806-1:— [2] and EN 13806-2:— [3]. All three
methods were validated in parallel in collaborative 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 (Hg) in foodstuffs using direct
atomic absorption spectrometry after thermal decomposition in an oxygen or air flow and
concentration by amalgam formation. The method is applicable for solid and liquid samples.
This method was tested in a collaborative study carried out on seven different materials with a mercury
concentration in the range from 0,005 mg/kg to 5,20 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 13804:2013, Foodstuffs - Determination of elements and their chemical species - General
considerations and specific requirements
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:
— IEC Electropedia: available at https://www.electropedia.org/
— ISO Online browsing platform: available at https://www.iso.org/obp
4 Principle
The samples to be analysed are weighed directly - without pressure digestion - into suitable sample
containers and are thermally decomposed in the analyser system in an oxygen atmosphere at approx.
700 °C. The resulting reaction gases are catalytically cleaned together with the mercury vapour, and the
mercury is concentrated on a consecutive amalgamator. Subsequently, the mercury is released as
atomic vapour by fast heating up of the amalgamator, transferred into a system of measurement
cuvettes and quantified by absorption at 253,7 nm.
By the simultaneous use of measurement cuvettes of different lengths, a dynamic measurement range
over several orders of magnitude can be achieved.
The total content of mercury is understood as the content measured using this document. It is indicated
in mg/kg.
WARNING 1 — 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 Stabilization
The standard, calibration and zero-point solutions are stabilized with hydrochloric acid (5.2). It is
recommended to adjust the hydrochloric acid concentration to approx. ω = 1 % in the solutions.
Alternatively, other stabilizing reagents may be used (for details see the instructions of the instrument
manufacturer or [2]).
5.6 Mercury stock solution, e.g. ϱ = 1 000 mg/l.
The stock solution is commercially available. It is recommended to use certified stock solutions.
5.7 Mercury standard solution
The standard solution is prepared from the stock solution (5.6) by means of dilution (e.g. see Table 1).
For this purpose, fill approx. 5 ml of water into a 20 ml volum
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