SIST EN 17266:2020
(Main)Foodstuffs - Determination elements and their chemical species - Determination of organomercury in seafood by elemental mercury analysis
Foodstuffs - Determination elements and their chemical species - Determination of organomercury in seafood by elemental mercury analysis
This document describes a method for the determination of organomercury in seafood/fishery products by elemental mercury analysis. The method has been successfully valideted in an interlaboratory study with a working range from 0,013 mg/kg to 5,12 mg/kg (HORRAT values <2) in seafood/fishery products [1], [2]. The limit of quantification is approximately 0,010 mg/kg organomercury (referring to dry weight, expressed as mercury) [3], [4].
Organic species of mercury, other than monomethylmercury, are also extracted and thus determined with this method. However, in seafood/fishery products the contribution from organic species of mercury other than monomethylmercury is negligible.
Lebensmittel - Bestimmung von Elementen und ihren Verbindungen - Bestimmung von Organoquecksilber in Fisch- und Meeresfrüchten mit Feststoffquecksilberbestimmung
Dieses Dokument legt ein Verfahren zur Bestimmung von Organoquecksilber in Fisch und Meeresfrüchten durch Nutzung eines Quecksilber Feststoff Analysators fest. Das Verfahren wurde in einem Ringversuch an Austerngewebe, Muschelgewebe, Hummer Hepatopankreas, Hundshaileber und Thunfisch mit Mengen von 0,01 mg/kg bis 5 mg/kg (bezogen auf das Trockengewicht und als Quecksilber ausgedrückt) erfolgreich validiert [1], [2].
Die Bestimmungsgrenze liegt bei etwa 0,01 mg/kg Organoquecksilber[3], [4].
Andere organische Quecksilberspezies als Monomethylquecksilber werden ebenfalls extrahiert und somit mit diesem Verfahren bestimmt. Bei Fisch und Meeresfrüchten ist der Beitrag anderer organischer Quecksilberspezies neben Monomethylquecksilber jedoch vernachlässigbar.
Produits alimentaires - Dosage des éléments et de leurs espèces chimiques - Dosage du mercure organique dans les fruits de mer par analyse du mercure élémentaire
La présente Norme européenne spécifie une méthode de dosage du mercure organique dans les produits
de la mer par analyse du mercure élémentaire. La méthode a été validée au cours d’un essai
interlaboratoires sur du tissu d’huître, du tissu de moule, de l’hépatopancréas de homard, du foie de
roussette et du thon à des niveaux allant de 0,01 mg/kg à 5 mg/kg faisant référence au poids sec et
exprimés en tant que mercure [1], [2].
La limite de quantification est d’environ 0,01 mg/kg de mercure organique [3], [4].
Les espèces organiques du mercure, autres que le monométhylmercure, sont également extraites et ainsi
dosées avec cette méthode. Cependant, dans les produits de la mer, la contribution des espèces
organiques du mercure autres que le monométhylmercure est négligeable.
Živila - Določevanje elementov in njihovih kemijskih oblik - Določevanje organskih živosrebrovih spojin v morski hrani z analizo elementarnega živega srebra
Ta dokument opisuje metodo za določanje organskega živega srebra v morskih /ribiških proizvodih z elementarno analizo živega srebra. Metoda je bila uspešno potrjena v medlaboratorijski študiji z delovnim obsegom od 0,013 mg/kg do 5,12 mg/kg (vrednosti HORRAT < 2) v morskih sadežih/ribiških proizvodih [1], [2]. Meja količinskega določanja je približno 0,010 mg/kg organskega živega srebra (ki se navezuje na suho maso, izraženo kot živo srebro) [3], [4]. Organske vrste živega srebra, razen monometilnega živega srebra, se tudi ekstrahirajo in tako določijo s to metodo. Vendar pa je v morskih/ribiških proizvodih prispevek organskih vrst živega srebra, razen monometilnega živega srebra, zanemarljiv.
General Information
Buy Standard
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN 17266:2020
01-januar-2020
Živila - Določevanje elementov in njihovih kemijskih oblik - Določevanje organskih
živosrebrovih spojin v morski hrani z analizo elementarnega živega srebra
Foodstuffs - Determination elements and their chemical species - Determination of
organomercury in seafood by elemental mercury analysis
Lebensmittel - Bestimmung von Elementen und ihren Verbindungen - Bestimmung von
Organoquecksilber in Fisch- und Meeresfrüchten mit Feststoffquecksilberbestimmung
Produits alimentaires - Dosage des éléments et de leurs espèces chimiques - Dosage du
mercure organique dans les fruits de mer par analyse du mercure élémentaire
Ta slovenski standard je istoveten z: EN 17266:2019
ICS:
67.120.30 Ribe in ribji proizvodi Fish and fishery products
SIST EN 17266:2020 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN 17266:2020
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SIST EN 17266:2020
EN 17266
EUROPEAN STANDARD
NORME EUROPÉENNE
November 2019
EUROPÄISCHE NORM
ICS 67.120.30
English Version
Foodstuffs - Determination elements and their chemical
species - Determination of organomercury in seafood by
elemental mercury analysis
Produits alimentaires - Dosage des éléments et de leurs Lebensmittel - Bestimmung von Elementen und ihren
espèces chimiques - Dosage du mercure organique Verbindungen - Bestimmung von Organoquecksilber in
dans les produits de la mer par analyse du mercure Fisch und Meeresfrüchten mittels Elementaranalyse
élémentaire von Quecksilber
This European Standard was approved by CEN on 9 September 2019.
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, Turkey 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
© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17266:2019 E
worldwide for CEN national Members.
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SIST EN 17266:2020
EN 17266:2019 (E)
Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 4
5 Reagents . 5
6 Apparatus and equipment . 8
7 Procedure. 8
7.1 Sample preparation . 8
7.2 Reagent blank solution . 8
7.3 Determination by elemental mercury analyser . 8
7.4 Instrumental parameters . 9
7.5 Analytical sequence . 9
8 Quality control . 9
8.1 Recovery . 9
8.2 Instrument verification . 10
8.3 Calibration curve . 10
8.4 Absence of contamination . 11
9 Evaluation . 11
9.1 Calculation . 11
9.2 Expression of results . 11
10 Precision . 11
10.1 General . 11
10.2 Repeatability . 11
10.3 Reproducibility . 11
11 Test report . 12
Annex A (informative) Precision data . 13
Bibliography . 15
2
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SIST EN 17266:2020
EN 17266:2019 (E)
European foreword
This document (EN 17266:2019) 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 May 2020, and conflicting national standards shall be
withdrawn at the latest by May 2020.
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.
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, Turkey and the
United Kingdom.
3
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SIST EN 17266:2020
EN 17266:2019 (E)
1 Scope
This document specifies a method for the determination of organomercury in seafood by elemental
mercury analysis. The method has been successfully validated in an interlaboratory study on oyster
tissue, mussel tissue, lobster hepatopancreas, dogfish liver and tuna at levels from 0,01 mg/kg to
5 mg/kg referring to dry weight and expressed as mercury [1], [2].
The limit of quantification is approximately 0,01 mg/kg of organomercury [3], [4].
Organic species of mercury, other than monomethylmercury, are also extracted and thus determined
with this method. However, in seafood the contribution from organic species of mercury other than
monomethylmercury is negligible.
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 ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696)
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at http://www.iso.org/obp
— IEC Electropedia: available at http://www.electropedia.org/
4 Principle
Organomercury in seafood/fishery products is separated from the matrix by double liquid-liquid
extraction, first with an organic solvent (toluene) and subsequently with L-cysteine solution and is
determined by elemental mercury analyser [3], [4].
Elemental mercury analyser, also known as automated or direct mercury analyser, is a single purpose
atomic absorption spectrophotometer for mercury determination. The determination of mercury with
an elemental mercury analyser is based on sample drying and subsequent thermal decomposition,
including electro thermal atomisation of mercury. A gold amalgamator selectively traps and pre-
concentrates the mercury from the flow of decomposition products. Finally, the trapped mercury is
thermally released and detected by atomic absorption at 253,7 nm. Organomercury results are
expressed in mg/kg as mercury.
Alternative detection techniques can be used, provided that equivalence of method performance is
proven.
4
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SIST EN 17266:2020
EN 17266:2019 (E)
5 Reagents
The mass concentration of mercury in the reagents and water used shall be low enough not to affect the
results. All reagents shall be of analytical grade, i.e. pro analysis, p.a. or similar unless otherwise
specified.
Use water conforming to grade 2 of EN ISO 3696.
5.1 Nitric acid, mass fraction, w (HNO ) = 65 % (m/m), density approximately 1,4 g/ml
3
5.2 Hydrochloric acid, w (HCl) = 32 % (m/m), density approximately 1,18 g/ml
5.3 Diluted hydrochloric acid solution
Mix equal volumes of hydrochloric acid (5.2) and water.
5.4 Hydrobromic acid, w (HBr) approximately 47 %, density approximately 1,47 g/ml
5.5 Toluene
1)
5.6 L-cysteine monohydrate hydrochloride, e.g. Ph. Eur. or USP grade
5.7 Sodium sulfate anhydrous
5.8 Sodium acetate anhydrous
5.9 L-cysteine solution, mass concentration ρ = 1 g/100 ml
Weigh 1,0 g of L-cysteine monohydrate hydrochloride (5.6), 12,5 g of sodium sulfate (5.7) and 0,8 g of
sodium acetate (5.8) into a 100 ml beaker. Add about 75 ml of water and stir until complete dissolution.
Transfer this solution completely to a 100 ml volumetric flask and make up to volume with water. This
solution can be stored for 1 day at ambient temperature. Other preparation volumes may be used as
long as proportions are kept.
The mass concentration of mercury in the L-cysteine solution should be as low as possible. The purity of
this solution should be such that the response for mercury shall be less than half the response of the
1 µg/l mercury standard solution (calibration solution 1, see 5.13).
L-cysteine precipitates on the catalytic tube which should thus be changed or cleaned as appropriate.
5.10 Mercury stock solution, ρ(Hg) = 1 000 mg/l Hg
5.11 Monomethylmercury (MMHg) chloride, minimum purity of 95 %
5.12 Mercury standard solutions
5.12.1 Mercury standard solution 1 (ρ = 10 mg/l Hg)
Pipette 1,0 ml of the commercial mercury stock solution 1 000 mg/l Hg (5.10) in a 100 ml volumetric
flask, add 2,0 ml of diluted hydrochloric acid solution (5.3) and make up to volume with water. This
solution is stable in a glass container in the refrigerator at approximately 2 °C to 10 °C for 6 months.
5.12.2 Mercury standard solution 2 (ρ = 0,50 mg/l Hg)
1)
Ph. Eur. = European Pharmacopoeia; USP = United States Pharmacopoeia.
5
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SIST EN 17266:2020
EN 17266:2019 (E)
Pipette 2,5 ml of mercury standard solution 1 (5.12.1) in a 50 ml volumetric flask, add 1,0 ml of diluted
hydrochloric acid solution (5.3) and make up to volume with water. This solution is stable in a glass
container in the refrigerator at approximately 2 °C to 10 °C for 2 months.
5.13 Calibration solutions
Due to the highly stable response of elemental mercury analysers, there is no need to recalibrate for
each analytical sequence. Calibration is usually stable for at least 1 year. For that reason every
instrumental calibration will be maintained for that period, provided that quality controls for each
sequence are satisfactory. Nevertheless, if the gold amalgamator or catalyst tube is changed, response
could change and a new calibration is necessary. In such a case, analyse 500 µl of each calibration
solution (from blank to 100 µg/l Hg). For selection of corresponding calibration solutions for each
calibration curve, see 7.4. For acceptance criteria regarding the calibration curve, see 8.3.
Select calibration solutions depending on the cell used, thus on the expected concentration level of the
sample. This is comprehensively described in 7.4.
Prepare all calibration solutions freshly for each calibration.
Other volumes of preparation are suitable provided that they maintain the proportions described
below. Pipette either mercury standard solution 2 (5.12.2) or calibration solution 7 (see Table 1) in a
50 ml volumetric flask and fill up to the mark with L-cysteine solution (5.9) according to the scheme
presented in Table 1.
Use L-cysteine solution (5.9) as blank (level 0) for calibration.
Table 1 — Example of calibration solutions
Volume of initial Final Hg
Calibration solution
solution concentration (ρ)
Initial solution
no
ml µg/l
0 L-cysteine solution (5.9) 50 0
1 calibration solution no 7 1,0 1,0
2 calibration solution no 7 2,5 2,5
3 standard solution 2 (5.12.2) 0,5 5,0
4 standard solution 2 (5.12.2) 1,0 10
5 standard solution 2 (5.12.2) 1,5 15
6 standard solution 2 (5.12.2) 2,5 25
7 standard solution 2 (5.12.2) 5,0 50
8 standard solution 2 (5.12.2) 7,5 75
9 standard solution 2 (5.12.2) 10,0 100
6
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SIST EN 17266:2020
EN 17266:2019 (E)
5.14 Internal quality control solutions
5.14.1 General
As the response of elemental mercury analysers is highly stable, there is no need to recalibrate the
instrument for each analytical sequence. However, some control solutions are used to ensure the
validity of the latest calibration. Each calibration curve needs to be compared against an external
solution to demonstrate absence of error in intermediate calibration s
...
SLOVENSKI STANDARD
SIST EN 17266:2020
01-januar-2020
Živila - Določevanje elementov in njihovih kemijskih oblik - Določevanje organskih
živosrebrovih spojin v morski hrani z analizo elementarnega živega srebra
Foodstuffs - Determination elements and their chemical species - Determination of
organomercury in seafood by elemental mercury analysis
Lebensmittel - Bestimmung von Elementen und ihren Verbindungen - Bestimmung von
Organoquecksilber in Fisch- und Meeresfrüchten mit Feststoffquecksilberbestimmung
Produits alimentaires - Dosage des éléments et de leurs espèces chimiques - Dosage du
mercure organique dans les fruits de mer par analyse du mercure élémentaire
Ta slovenski standard je istoveten z: EN 17266:2019
ICS:
67.120.30 Ribe in ribji proizvodi Fish and fishery products
SIST EN 17266:2020 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN 17266:2020
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SIST EN 17266:2020
EN 17266
EUROPEAN STANDARD
NORME EUROPÉENNE
November 2019
EUROPÄISCHE NORM
ICS 67.120.30
English Version
Foodstuffs - Determination elements and their chemical
species - Determination of organomercury in seafood by
elemental mercury analysis
Produits alimentaires - Dosage des éléments et de leurs Lebensmittel - Bestimmung von Elementen und ihren
espèces chimiques - Dosage du mercure organique Verbindungen - Bestimmung von Organoquecksilber in
dans les produits de la mer par analyse du mercure Fisch und Meeresfrüchten mittels Elementaranalyse
élémentaire von Quecksilber
This European Standard was approved by CEN on 9 September 2019.
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, Turkey 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
© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17266:2019 E
worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST EN 17266:2020
EN 17266:2019 (E)
Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 4
5 Reagents . 5
6 Apparatus and equipment . 7
7 Procedure. 8
7.1 Sample preparation . 8
7.2 Reagent blank solution . 8
7.3 Determination by elemental mercury analyser . 8
7.4 Instrumental parameters . 9
7.5 Analytical sequence . 9
8 Quality control . 9
8.1 Recovery . 9
8.2 Instrument verification . 10
8.3 Calibration curve . 10
8.4 Absence of contamination . 11
9 Evaluation . 11
9.1 Calculation . 11
9.2 Expression of results . 11
10 Precision . 11
10.1 General . 11
10.2 Repeatability . 11
10.3 Reproducibility . 11
11 Test report . 12
Annex A (informative) Precision data . 13
Bibliography . 15
2
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SIST EN 17266:2020
EN 17266:2019 (E)
European foreword
This document (EN 17266:2019) 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 May 2020, and conflicting national standards shall be
withdrawn at the latest by May 2020.
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.
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, Turkey and the
United Kingdom.
3
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SIST EN 17266:2020
EN 17266:2019 (E)
1 Scope
This document specifies a method for the determination of organomercury in seafood by elemental
mercury analysis. The method has been successfully validated in an interlaboratory study on oyster
tissue, mussel tissue, lobster hepatopancreas, dogfish liver and tuna at levels from 0,01 mg/kg to
5 mg/kg referring to dry weight and expressed as mercury [1], [2].
The limit of quantification is approximately 0,01 mg/kg of organomercury [3], [4].
Organic species of mercury, other than monomethylmercury, are also extracted and thus determined
with this method. However, in seafood the contribution from organic species of mercury other than
monomethylmercury is negligible.
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 ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696)
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at http://www.iso.org/obp
— IEC Electropedia: available at http://www.electropedia.org/
4 Principle
Organomercury in seafood/fishery products is separated from the matrix by double liquid-liquid
extraction, first with an organic solvent (toluene) and subsequently with L-cysteine solution and is
determined by elemental mercury analyser [3], [4].
Elemental mercury analyser, also known as automated or direct mercury analyser, is a single purpose
atomic absorption spectrophotometer for mercury determination. The determination of mercury with
an elemental mercury analyser is based on sample drying and subsequent thermal decomposition,
including electro thermal atomisation of mercury. A gold amalgamator selectively traps and pre-
concentrates the mercury from the flow of decomposition products. Finally, the trapped mercury is
thermally released and detected by atomic absorption at 253,7 nm. Organomercury results are
expressed in mg/kg as mercury.
Alternative detection techniques can be used, provided that equivalence of method performance is
proven.
4
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SIST EN 17266:2020
EN 17266:2019 (E)
5 Reagents
The mass concentration of mercury in the reagents and water used shall be low enough not to affect the
results. All reagents shall be of analytical grade, i.e. pro analysis, p.a. or similar unless otherwise
specified.
Use water conforming to grade 2 of EN ISO 3696.
5.1 Nitric acid, mass fraction, w (HNO ) = 65 % (m/m), density approximately 1,4 g/ml
3
5.2 Hydrochloric acid, w (HCl) = 32 % (m/m), density approximately 1,18 g/ml
5.3 Diluted hydrochloric acid solution
Mix equal volumes of hydrochloric acid (5.2) and water.
5.4 Hydrobromic acid, w (HBr) approximately 47 %, density approximately 1,47 g/ml
5.5 Toluene
1)
5.6 L-cysteine monohydrate hydrochloride, e.g. Ph. Eur. or USP grade
5.7 Sodium sulfate anhydrous
5.8 Sodium acetate anhydrous
5.9 L-cysteine solution, mass concentration ρ = 1 g/100 ml
Weigh 1,0 g of L-cysteine monohydrate hydrochloride (5.6), 12,5 g of sodium sulfate (5.7) and 0,8 g of
sodium acetate (5.8) into a 100 ml beaker. Add about 75 ml of water and stir until complete dissolution.
Transfer this solution completely to a 100 ml volumetric flask and make up to volume with water. This
solution can be stored for 1 day at ambient temperature. Other preparation volumes may be used as
long as proportions are kept.
The mass concentration of mercury in the L-cysteine solution should be as low as possible. The purity of
this solution should be such that the response for mercury shall be less than half the response of the
1 µg/l mercury standard solution (calibration solution 1, see 5.13).
L-cysteine precipitates on the catalytic tube which should thus be changed or cleaned as appropriate.
5.10 Mercury stock solution, ρ(Hg) = 1 000 mg/l Hg
5.11 Monomethylmercury (MMHg) chloride, minimum purity of 95 %
5.12 Mercury standard solutions
5.12.1 Mercury standard solution 1 (ρ = 10 mg/l Hg)
Pipette 1,0 ml of the commercial mercury stock solution 1 000 mg/l Hg (5.10) in a 100 ml volumetric
flask, add 2,0 ml of diluted hydrochloric acid solution (5.3) and make up to volume with water. This
solution is stable in a glass container in the refrigerator at approximately 2 °C to 10 °C for 6 months.
5.12.2 Mercury standard solution 2 (ρ = 0,50 mg/l Hg)
1)
Ph. Eur. = European Pharmacopoeia; USP = United States Pharmacopoeia.
5
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SIST EN 17266:2020
EN 17266:2019 (E)
Pipette 2,5 ml of mercury standard solution 1 (5.12.1) in a 50 ml volumetric flask, add 1,0 ml of diluted
hydrochloric acid solution (5.3) and make up to volume with water. This solution is stable in a glass
container in the refrigerator at approximately 2 °C to 10 °C for 2 months.
5.13 Calibration solutions
Due to the highly stable response of elemental mercury analysers, there is no need to recalibrate for
each analytical sequence. Calibration is usually stable for at least 1 year. For that reason every
instrumental calibration will be maintained for that period, provided that quality controls for each
sequence are satisfactory. Nevertheless, if the gold amalgamator or catalyst tube is changed, response
could change and a new calibration is necessary. In such a case, analyse 500 µl of each calibration
solution (from blank to 100 µg/l Hg). For selection of corresponding calibration solutions for each
calibration curve, see 7.4. For acceptance criteria regarding the calibration curve, see 8.3.
Select calibration solutions depending on the cell used, thus on the expected concentration level of the
sample. This is comprehensively described in 7.4.
Prepare all calibration solutions freshly for each calibration.
Other volumes of preparation are suitable provided that they maintain the proportions described
below. Pipette either mercury standard solution 2 (5.12.2) or calibration solution 7 (see Table 1) in a
50 ml volumetric flask and fill up to the mark with L-cysteine solution (5.9) according to the scheme
presented in Table 1.
Use L-cysteine solution (5.9) as blank (level 0) for calibration.
Table 1 — Example of calibration solutions
Volume of initial Final Hg
Calibration solution
solution concentration (ρ)
Initial solution
no
ml µg/l
0 L-cysteine solution (5.9) 50 0
1 calibration solution no 7 1,0 1,0
2 calibration solution no 7 2,5 2,5
3 standard solution 2 (5.12.2) 0,5 5,0
4 standard solution 2 (5.12.2) 1,0 10
5 standard solution 2 (5.12.2) 1,5 15
6 standard solution 2 (5.12.2) 2,5 25
7 standard solution 2 (5.12.2) 5,0 50
8 standard solution 2 (5.12.2) 7,5 75
9 standard solution 2 (5.12.2) 10,0 100
6
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EN 17266:2019 (E)
5.14 Internal quality control solutions
5.14.1 General
As the response of elemental mercury analysers is highly stable, there is no need to recalibrate the
instrument for each analytical sequence. However, some control solutions are used to ensure the
validity of the latest calibration. Each calibration curve needs to be compared against an external
solution to demonstrate absence of error in intermediate calibration solutions preparation.
...
SLOVENSKI STANDARD
oSIST prEN 17266:2018
01-oktober-2018
äLYLOD'RORþHYDQMHHOHPHQWRYLQQMLKRYLKNHPLMVNLKREOLN'RORþHYDQMH
åLYRVUHEURYLKRUJDQVNLKVSRMLQYPRUVNLKVDGHåLK]DQDOL]RHOHPHQWDUQHJDåLYHJD
VUHEUD
Foodstuffs - Determination elements and their chemical species - Determination of
organomercury in seafood by elemental mercury analysis
Lebensmittel - Bestimmung von Elementen und ihren Verbindungen - Bestimmung von
Organoquecksilber in Fisch- und Meeresfrüchten mit Feststoffquecksilberbestimmung
Produits alimentaires - Dosage des éléments et de leurs espèces chimiques - Dosage du
mercure organique dans les fruits de mer par analyse du mercure élémentaire
Ta slovenski standard je istoveten z: prEN 17266
ICS:
67.120.30 Ribe in ribji proizvodi Fish and fishery products
oSIST prEN 17266:2018 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN 17266:2018
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oSIST prEN 17266:2018
DRAFT
EUROPEAN STANDARD
prEN 17266
NORME EUROPÉENNE
EUROPÄISCHE NORM
July 2018
ICS 67.120.30
English Version
Foodstuffs - Determination elements and their chemical
species - Determination of organomercury in seafood by
elemental mercury analysis
Produits alimentaires - Dosage des éléments et de leurs Lebensmittel - Bestimmung von Elementen und ihren
espèces chimiques - Dosage du mercure organique Verbindungen - Bestimmung von Organoquecksilber in
dans les fruits de mer par analyse du mercure Fisch- und Meeresfrüchten mit
élémentaire Feststoffquecksilberbestimmung
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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey 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
© 2018 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 17266:2018 E
worldwide for CEN national Members.
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prEN 17266:2018 (E)
Contents
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 4
5 Reagents . 4
6 Apparatus and equipment . 7
7 Procedure . 8
7.1 Sample preparation . 8
7.2 Reagent blank solution . 8
7.3 Determination by elemental mercury analyser . 8
7.4 Instrumental parameters . 8
7.5 Analytical sequence . 9
8 Quality control . 9
8.1 Recovery . 9
8.2 Instrument verification . 10
8.3 Calibration curve . 10
8.4 Absence of contamination . 10
9 Evaluation . 11
9.1 Calculation . 11
9.2 Expression of results . 11
10 Precision . 11
10.1 General . 11
10.2 Repeatability . 11
10.3 Reproducibility . 11
11 Test report . 12
Annex A (informative) Precision data . 13
Bibliography . 14
2
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prEN 17266:2018 (E)
European foreword
This document (prEN 17266:2018) 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.
3
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1 Scope
This document describes a method for the determination of organomercury in seafood/fishery
products by elemental mercury analysis. The method has been successfully valideted in an
interlaboratory study with a working range from 0,013 mg/kg to 5,12 mg/kg (HORRAT values < 2) in
seafood/fishery products [1], [2]. The limit of quantification is approximately 0,010 mg/kg
organomercury (referring to dry weight, expressed as mercury) [3], [4].
Organic species of mercury, other than monomethylmercury, are also extracted and thus determined
with this method. However, in seafood/fishery products the contribution from organic species of
mercury other than monomethylmercury is negligible.
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 ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696)
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
• IEC Electropedia: available at http://www.electropedia.org/
• ISO Online browsing platform: available at http://www.iso.org/obp
4 Principle
Organomercury in seafood/fishery products is separated from the matrix by double liquid-liquid
extraction, first with an organic solvent (toluene) and subsequently with L-cysteine solution and is
detected and determined by elemental mercury analyser [3], [4].
Elemental mercury analyser, also known as automated or direct mercury analyser, is a single purpose
atomic absorption spectrophotometer for mercury determination. The determination of mercury with
an elemental mercury analyser is based on sample drying and subsequent thermal decomposition,
followed by electro thermal atomisation of mercury. A gold amalgamator selectively traps and pre-
concentrates the mercury from the flow of decomposition products. Finally, the trapped mercury is
thermally released and detected by atomic absorption at 253,7 nm. Organomercury results are
expressed in mg/kg as mercury.
The sample solution can be detected with alternative detection techniques provided that equivalence of
method performance is proven.
5 Reagents
The mass concentration of mercury in the reagents and water used shall be low enough not to affect the
results. All reagents shall be of analytical grade, i.e. pro analysi, p.a. or similar unless otherwise
specified.
Use water conforming to grade 2 of EN ISO 3696.
4
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1)
5.1 Nitric acid, minimum w = 65 % , density about 1,4 g/ml
2)
5.2 Hydrochloric acid, minimum w = 32 %, p. a., ρ = 1,18 g/ml
5.3 Diluted hydrochloric acid solution,
Mix equal volumes of hydrochloric acid (5.2) and water.
5.4 Hydrobromic acid, w = 47 %, p. a., ρ = 1,47 g/ml
5.5 Toluene, p. a.
3)
5.6 L-cysteine monohydrate hydrochloride, Ph. Eur. or USP grade
5.7 Sodium sulfate anhydrous, p. a.
5.8 Sodium acetate anhydrous
5.9 L-cysteine solution, ρ = 1 g/100 ml
Weigh (6.3) 1,0 g of L-cysteine monohydrate hydrochloride, 1,25 g of sodium sulfate (5.7) and 0,8 g of
sodium acetate (5.8) into a 100 ml beaker. Add about 75 ml of water and stir until complete dissolution.
Transfer this solution completely to a 100 ml volumetric flask and make up to volume with water. This
solution can be stored for 1 day at ambient temperature. Other preparation volumes may be used as
long as proportions are kept.
The mass concentration of mercury in the L-cysteine solution should be as low as possible. The purity of
this solution should be such that the response for mercury shall be less than half the response of the
1 µg/l mercury standard solution (calibration solution 9, see 5.13.1).
5.10 Mercury reference solution, of 1 000 mg/l Hg
5.11 Monomethylmercury (MMHg) chloride, minimum purity of 95 %
5.12 Mercury stock solutions
5.12.1 Stock solution 1 (ρ = 10 mg/l Hg)
Pipette 1,00 ml of the commercial mercury reference solution 1 000 mg/l Hg (5.10) in a 100 ml
volumetric flask; add 2 ml of diluted hydrochloric acid solution (5.3) and make up to volume with
water. This solution is stable in a glass container in the refrigerator at approximately 2 °C to 10 °C for
6 months.
5.12.2 Stock solution 2 (ρ = 500 µg/l Hg)
Pipette 2,50 ml of stock solution 1 (5.12.1) in a 50 ml volumetric flask, add 1 ml of diluted hydrochloric
acid solution (5.3) and make up to volume with water. This solution is stable in a glass container in the
refrigerator at approximately 2 °C to 10 °C for 2 months.
1)
w = mass fraction.
2)
ρ = mass concentration.
3)
Ph. Eur. = European Pharmacopoeia; USP = United Stated Pharmacopoeia.
5
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5.13 Calibration solutions
5.13.1 Mercury calibration solutions
Due to the highly stable response of elemental mercury analysers, there is no need to recalibrate for
each analytical sequence. Calibration is usually stable for at least 1 year. For that reason every
instrumental calibration will be maintained for that period, provided that quality controls for each
sequence are satisfactory. Nevertheless, if the gold amalgamator or catalyst tube is changed, response
could change and a new calibration is necessary . In such a case, analyse 500 µl of each calibration
solution (from blank to 100 µg/l Hg). for selection of corresponding standard solutions for each
calibration curve, see 6.4. or acceptance criteria regarding the calibration curve, see 7.3.
Select calibration standard solutions depending on the cell used, thus on the expected concentration
level of the sample. This is comprehensively described in 6.4.
Prepare all calibration standard solutions freshly for each calibration. Other volumes of preparation are
suitable provided that they maintain the proportions described below.
Prepare calibration standard solutions from either the stock solution 2 (5.12.2) or the
calibration solution 3 (see Table 1), placed into a 50 ml volumetric flask and filled up to the mark with
L-cysteine solution (5.9) according to the scheme presented in Table 1.
Table 1 — Example of mercury calibration standard solutions
Quantity of initial Final Hg
Calibration standard
solution concentration (ρ)
Initial solution
solution no
ml µg/l
1 stock solution 2 (5.12.2) 10 100
2 stock solution 2 (5.12.2) 7,5 75
3 stock solution 2 (5.12.2) 5,0 50
4 stock solution 2 (5.12.2) 2,5 25
5 stock solution 2 (5.12.2) 1,5 15
6 stock solution 2 (5.12.2) 1,0 10
7 stock solution 2 (5.12.2) 0,5 5,0
8 calibration solution no 3 2,5 2,5
9 calibration solution no 3 1,0 1,0
5.13.2 Blank solution for calibration
Use L-cysteine 1 % (w/v) solution (5.9) as blank (level 0) for instrumental calibration.
5.14 Internal quality control solutions
5.14.1 General
As the response of elemental mercury analysers is highly stable, there is no need to recalibrate the
instrument for each analytical sequence. However, some control solutions are used to ensure the
validity of the latest calibration. Each calibration curve needs to be compared against an external
solution to demonstrate absence of error in intermediate standard solutions preparation.
6
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Quality control solution 2 (QC2) ensures that quantification at low level is st
...
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