EN 17053:2018
(Main)Animal feeding stuffs: Methods of sampling and analysis - Determination of trace elements, heavy metals and other elements in feed by ICP-MS (multi-method)
Animal feeding stuffs: Methods of sampling and analysis - Determination of trace elements, heavy metals and other elements in feed by ICP-MS (multi-method)
This European Standard specifies a method for the determination of trace elements, heavy metals and other elements in animal feed by inductively coupled plasma mass spectrometry (ICP-MS). The method is used to determine As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, Tl, U and Zn in the extraction solution after pressurized digestion. For the determination of extractable lead in minerals and feeds containing phyllosilicates (e.g. kaolinite clay) wet digestion with nitric acid should be used. The method described is suitable for use in quadrupole instruments equipped either with or without additional technology to reduce molecular ion interferences (e.g. collision or reaction technologies) as well as in high-resolution sector-field systems.
The method was fully statistically tested and evaluated in a collaborative trial comprising eight animal feeding stuff samples for the elements As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, Tl, U and Zn. For elements with a HORRAT value higher than 2 (e.g. mercury, see Annex A) the method is more applicable as a screening method and not for confirmatory purposes. High-resolution sector-field ICP-MS was not tested in the validation ring trial.
The limit of quantification for each element is dependent on the sample matrix as well as the instrument. For the elements Co, Mn, Mo, Pb, Tl, U a limit of quantification of 0,10 mg/kg should normally be obtained, for the elements Fe and Zn 5,0 mg/kg, while for Cd 0,03 mg/kg, Hg 0,04 mg/kg and As 0,05 mg/kg should normally be quantifiable.
Details on the successfully tested working range for each element are described in this standard.
Futtermittel - Probenahme- und Untersuchungsverfahren - Bestimmung von Spurenelementen, Schwermetallen und anderen Elementen in Futtermitteln mittels ICP-MS (Multimethode)
Diese Europäische Norm legt ein Verfahren zur Bestimmung von Spurennährstoffen, Schwermetallen und anderen Elementen in Tierfuttermitteln durch Massenspektrometrie mit induktiv gekoppeltem Plasma (ICP MS) fest. Das Verfahren wird zur Bestimmung von As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, Tl, U und Zn in der Extraktionslösung nach Druckaufschluss verwendet. Zur Bestimmung von extrahierbarem Blei in Mineralstoffen und Futtermitteln, die Schichtsilikate enthalten (z. B. kaolinitischer Ton), sollte Nassaufschluss mit Salpetersäure verwendet werden. Das beschriebene Verfahren ist zur Verwendung mit Quadrupol Instrumenten geeignet, die entweder mit oder ohne zusätzliche Technologien zur Reduzierung der Interferenzen von Molekülionen (z. B. Kollisions oder Reaktionstechnologien) sowie hochauflösende Sektorfeldsysteme ausgestattet sind.
Das Verfahren wurde vollständig im Rahmen eines Ringversuches mit acht Futtermittelproben für die Elemente As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, Tl, U und Zn statistisch geprüft und bewertet. Für Elemente mit einem HorRat Wert höher als 2 (z. B. Quecksilber, siehe Anhang A) ist das Verfahren eher als Screening Verfahren und nicht für Bestätigungszwecke geeignet Eine ICP MS mit hochauflösendem Sektorfeldsystem wurde im Rahmen des Ringversuches nicht geprüft.
Die Nachweisgrenze des Verfahrens hängt bei jedem Element sowohl von der Probenmatrix als auch vom verwendeten Gerät ab. Für die Elemente Co, Mn, Mo, Pb, Tl und U sollte eine Bestimmungsgrenze von 0,10 mg/kg, für die Elemente Fe und Zn 5,0 mg/kg, für Cd 0,03 mg/kg, für Hg 0,04 mg/kg und für As 0,05 mg/kg üblicherweise quantifizierbar sein.
Nähere Angaben zu den erfolgreich geprüften Arbeitsbereichen für jedes Element werden in dieser Norm beschrieben.
Aliments des animaux - Méthodes d'échantillonnage et d'analyse - Dosage par ICP-MS (multiméthode) des éléments traces, métaux lourds et autres éléments inorganiques présents dans les aliments
Krma: metode vzorčenja in analize - Določevanje elementov v sledovih, težkih kovin in drugih elementov v krmi z ICP-MS (večelementna metoda)
Ta evropski standard določa metodo za določanje elementov v sledovih, težkih kovin in drugih elementov v živalski krmi po ICP-MS. Metoda se uporablja za določanje As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, Tl, U in Zn v raztopini za izločanje po razgradnji pod tlakom. Za določevanje izločljivega svinca v mineralih in krmah, ki vsebujejo filosilikate (npr. kaolinitna glina), je treba uporabiti postopek mokrega razklopa z dušikovo kislino. Opisana metoda je primerna za uporabo pri kvadrupolnih instrumentih, opremljenih z dodatno tehnologijo za zmanjševanje motenj molekularnih ionov (npr. tehnologije trkov ali reakcij) ali brez te tehnologije, ter pri visokoločljivostnih sistemih sektorskih polj.
Metoda je bila v celoti statistično preskušena in ocenjena v medlaboratorijskem poskusu, sestavljenem iz osmih vzorcev živalske krme za elemente As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, Tl, U in Zn. Visokoločljivostni ICP-MS za sektorsko polje ni bil preskušen pri primerjalnem preskusu za validacijo.
Meja kvantifikacije vseh elementov je odvisna od matrice vzorca in instrumenta. Pri elementih Co, Mn, Mo, Pb, Tl, U naj bi se običajno pridobila meja kvantifikacije 0,10 mg/kg, za elementa Fe in Zn 5,0 mg/kg, za Cd pa naj bi se običajno pridobila meja 0,03 mg/kg, za Hg 0,04 mg/kg in za As 0,05 mg/kg.
Podrobnosti o uspešno preskušenem delovnem razponu za posamezen element so opisane v tem standardu.
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
01-marec-2018
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Animal feeding stuffs: Methods of sampling and analysis - Determination of trace
elements, heavy metals and other elements in feed by ICP-MS (multi-method)
Futtermittel - Probenahme- und Untersuchungsverfahren - Bestimmung von
Spurenelementen, Schwermetallen und anderen Elementen in Futtermitteln mittels ICP-
MS (Multimethode)
Aliments des animaux - Méthodes d'échantillonnage et d'analyse - Dosage par ICP-MS
(multiméthode) des éléments traces, métaux lourds et autres éléments inorganiques
présents dans les aliments
Ta slovenski standard je istoveten z: EN 17053:2018
ICS:
65.120 Krmila Animal feeding stuffs
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EN 17053
EUROPEAN STANDARD
NORME EUROPÉENNE
January 2018
EUROPÄISCHE NORM
ICS 65.120
English Version
Animal feeding stuffs: Methods of sampling and analysis -
Determination of trace elements, heavy metals and other
elements in feed by ICP-MS (multi-method)
Aliments des animaux - Méthodes d'échantillonnage et Futtermittel - Probenahme- und
d'analyse - Dosage par ICP-MS (multiméthode) des Untersuchungsverfahren - Bestimmung von
éléments traces, métaux lourds et autres éléments Spurenelementen, Schwermetallen und anderen
inorganiques présents dans les aliments Elementen in Futtermitteln mittels ICP-MS
(Multimethode)
This European Standard was approved by CEN on 27 November 2017.
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, 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.
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. EN 17053:2018 E
worldwide for CEN national Members.
Contents Page
1 Scope . 4
2 Normative references . 4
3 Principle . 4
4 Reagents . 5
5 Apparatus . 6
6 Sampling . 6
7 Preparation and preservation of test samples . 6
7.1 General . 6
7.2 Animal feeding stuff, which can be ground as such . 7
7.3 Mineral animal feeding stuffs . 7
8 Procedure. 7
8.1 Pressure digestion . 7
8.2 Extractable lead in minerals and feeds containing phyllosilicates (e.g. kaolinite clay)
– extraction with diluted nitric acid . 7
8.3 Calibration . 8
8.4 Preparation of measurement solutions . 8
8.5 Determination . 9
8.6 Quality assurance . 12
9 Calculation . 12
10 Precision . 13
10.1 General . 13
10.2 Repeatability . 13
10.3 Reproducibility . 13
11 Test report . 13
Annex A (informative) Statistical results of interlaboratory tests (listed by element) . 14
Annex B (informative) Interferences . 27
B.1 Interferences in ICP-MS . 27
B.2 Technical solutions to overcome interferences . 28
Bibliography . 29
European foreword
This document (EN 17053:2018) has been prepared by Technical Committee CEN/TC 327 “Animal
feeding stuffs - Methods of sampling and analysis”, the secretariat of which is held by NEN.
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 July 2018, and conflicting national standards shall be
withdrawn at the latest by July 2018.
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 has been prepared under a mandate given to CEN by the European Commission and the
European Free Trade Association.
WARNING — The method described in this standard implies the use of reagents that pose a
hazard to health. The standard does not claim to address all associated safety problems. It is the
responsibility of the user of this standard to take appropriate measures for the health and safety
protection of the personnel prior to use of the standard and to ensure that regulatory and legal
requirements are complied with.
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, 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 the United Kingdom.
1 Scope
This European Standard specifies a method for the determination of trace elements, heavy metals and
other elements in animal feed by inductively coupled plasma mass spectrometry (ICP-MS). The method
is used to determine As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, Tl, U and Zn in the extraction solution after
pressurized digestion. For the determination of extractable lead in minerals and feeds containing
phyllosilicates (e.g. kaolinite clay) wet digestion with nitric acid should be used. The method described
is suitable for use in quadrupole instruments equipped either with or without additional technology to
reduce molecular ion interferences (e.g. collision or reaction technologies) as well as in high-resolution
sector-field systems.
The method was fully statistically tested and evaluated in a collaborative trial comprising eight animal
feeding stuff samples for the elements As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, Tl, U and Zn. For elements
with a HORRAT value higher than 2 (e.g. mercury, see Annex A) the method is more applicable as a
screening method and not for confirmatory purposes. High-resolution sector-field ICP-MS was not
tested in the validation ring trial.
The limit of quantification for each element is dependent on the sample matrix as well as the
instrument. For the elements Co, Mn, Mo, Pb, Tl, U a limit of quantification of 0,10 mg/kg should
normally be obtained, for the elements Fe and Zn 5,0 mg/kg, while for Cd 0,03 mg/kg, Hg 0,04 mg/kg
and As 0,05 mg/kg should normally be quantifiable.
Details on the successfully tested working range for each element are described in this standard.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
EN ISO 3696, Water for analytical laboratory use — Specification and test methods (ISO 3696)
EN ISO 6498, Animal feeding stuffs — Guidelines for sample preparation (ISO 6498)
3 Principle
For the determination of As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, Tl, U and Zn a test portion of the sample is
digested with concentrated nitric acid under pressure.
For the determination of extractable lead in minerals and feeds containing phyllosilicates (e.g. kaolinite
clay) wet digestion with nitric acid should be used.
The concentration of the elements is determined by inductively coupled plasma mass spectrometry
(ICP-MS) using external calibration or standard addition technique. To reduce occurring mass
interferences mathematical correction equations, physical or chemical technical solutions (see B.2) or
high-resolution sector-field ICP-MS may be applied.
4 Reagents
WARNING — The use of this European Standard can 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 European Standard to establish
appropriate safety and health practices and determine the applicability of regulatory limitations
prior to use.
Use only reagents of recognized analytical grade and water conforming to grade 2 of EN ISO 3696.
4.1 Nitric acid concentrated, not less than 65 % (mass fraction), c(HNO ) = 14,4 mol/l, having a
density of approximately ρ(HNO ) = 1,40 g/ml.
4.2 Nitric acid solution of 5 % (mass fraction), Pipette 54 ml of nitric acid (4.1) into a 1 000 ml
volumetric flask (5.4) and fill to the mark with water.
4.3 Nitric acid solution (rinsing solution), Pipette 20 ml nitric acid (4.1) in a 1 000 ml volumetric
flask (5.4). Fill up to the mark with water.
4.4 Hydrochloric acid concentrated, 30 % (mass fraction), c(HCl) = 9,5 mol/l, having a density of
approximately ρ(HCl) = 1,15 g/ml.
4.5 Hydrogen peroxide, not less than 30 % (mass fraction), c(H O ) = 9,7 mol/l, having a density
2 2
of approximately ρ(H O ) = 1,12 g/ml.
2 2
4.6 Single-element and multi-element stock solutions for ICP-MS, β = 1 000 mg/l, It is advisable
to use certified multi-element stock solutions. Stock solutions with concentrations different from
1 000 mg/l may be used as well. Stock solutions are considered to be stable for several months.
4.7 Calibration solutions, The concentrations of the calibration solutions depend on the element and
the estimated concentration levels in the samples. When preparing calibration solutions care should be
taken to pipette suitable volumes, intermediate dilution steps are recommended. If calibration solutions
are prepared from single-element stock solutions, it should be checked whether they are chemically
compatible and sufficiently pure (specification). Calibration solutions shall be prepared daily.
4.8 Internal standard stock solution, β = 1000 mg/l; As internal standard rhodium is
recommended.
NOTE Alternatively, for low mass
...
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