EN 15550:2017
(Main)Animal feeding stuffs: Methods of sampling and analysis - Determination of cadmium and lead by graphite furnace atomic absorption spectrometry (GF-AAS) after pressure digestion
Animal feeding stuffs: Methods of sampling and analysis - Determination of cadmium and lead by graphite furnace atomic absorption spectrometry (GF-AAS) after pressure digestion
This European Standard specifies a method for the determination of the elements cadmium and lead in animal feeding stuffs by graphite furnace atomic absorption spectrometry (GF-AAS) after pressure digestion.
The method was successfully tested in the range of 0,015 to 5,65 mg/kg for Cd and 0,18 to 40,3 mg/kg for lead in 11 animal feeds: 2 complete feeds (pig feed, sheep feed), 2 complementary feeds (2 mineral feeds), 1 mineral premixture, 4 feed materials (MgO, 2 phosphates, CaCO3) and 2 feed additives (CuSO4, bentonite).
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 limit of quantification for each element is dependent on the sample matrix as well as the instrument. For cadmium a limit of quantification of 0,05 mg/kg should normally be obtained while for lead, a limit of quantification of 0,5 mg/kg should be obtained.
Futtermittel - Probenahme und Untersuchungsverfahren - Bestimmung von Cadmium und Blei mittels Graphitrohrofen-Atomabsorptionsspektrometrie (GF-AAS) nach Druckaufschluss
Diese Europäische Norm legt ein Verfahren zur Bestimmung der Elemente Cadmium und Blei in Futtermitteln mit Graphitrohrofen-Atomabsorptionsspektrometrie (GF AAS) nach Druckaufschluss fest.
Das Verfahren wurde bei 11 Futtermitteln im Bereich von 0,015 bis 5,65 mg/kg für Cadmium und 0,18 bis 40,3 mg/kg für Blei erfolgreich geprüft: 2 Alleinfuttermittel (für Schweine und Schafe), 2 Ergänzungsfuttermittel (2 Mineralfutter), 1 Mineralstoffmischung, 4 Einsatzfuttermittel (MgO, 2-Phosphat, CaCO3) und 2 Futtermittel-Zusatzstoffe (CuSO4, Bentonit).
Zur Bestimmung von extrahierbarem Blei in Mineralien und Futtermitteln, die Schichtsilikate (z. B. Kaolinit Ton) enthalten, sollte Nassaufschluss mit Salpetersäure verwendet werden.
Die Nachweisgrenze des Verfahrens hängt bei jedem Element sowohl von der Probenmatrix als auch vom verwendeten Gerät ab. Für Cadmium sollte normalerweise eine Bestimmungsgrenze von 0,05 mg/kg erreicht werden, während für Blei eine Bestimmungsgrenze von 0,5 mg/kg erreicht werden sollte.
Aliments des animaux - Méthodes d'échantillonnage et d'analyse - Dosage du cadmium et du plomb par spectrométrie d'absorption atomique en four graphite (SAA-FG) après digestion sous pression
La présente Norme européenne spécifie une méthode de dosage des éléments cadmium et plomb dans les aliments pour animaux, par spectrométrie d’absorption atomique en four graphite (SAA-FG) après digestion sous pression.
Cette méthode a été mise en application de façon satisfaisante dans une gamme de 0,015 à 5,65 mg/kg pour le cadmium et de 0,18 à 40,3 mg/kg pour le plomb, en utilisant onze aliments pour animaux : deux aliments complets (un aliment pour porcs et un aliment pour ovins), deux aliments complémentaires (minéraux), un prémélange minéral, quatre matières premières destinées aux aliments pour animaux (MgO, deux phosphates, CaCO3), et deux additifs utilisés en alimentation animale (CuSO4, bentonite).
Pour doser le plomb extractible dans les minéraux et les aliments contenant des phyllosilicates (par exemple, de l'argile de kaolinite), il convient d'utiliser une méthode de minéralisation par voie humide à l'acide nitrique.
La limite de quantification de la méthode correspondant à chacun des éléments est fonction de la matrice de l'échantillon et de l'instrument. Il convient de parvenir à une limite de quantification de 0,05 mg/kg pour le cadmium et de 0,5 mg/kg pour le plomb.
Krma: metode vzorčenja in analize - Določevanje kadmija in svinca z atomsko absorpcijsko spektrometrijo (GF-AAS) z grafitno kiveto po razklopu pod tlakom
Ta evropski standard določa metodo za določevanje kadmija in svinca v krmi z atomsko absorpcijsko spektrometrijo (GF-AAS) z grafitno kiveto po razklopu pod tlakom.
Metoda je bila uspešno testirana v razponu od 0,015 do 5,65 mg/kg za kadmij in 0,18 do 40,3 mg/kg za svinec v enajstih krmah: dveh celovitih krmah (krmi za prašiče, krmi za ovce), dveh dopolnilnih krmah (dveh mineralnih krmah), enem mineralnem premiksu, štirih sestavinah krme (MgO, dveh fosfatih, CaCO3) in dveh dodatkih za krmo (CuSO4, bentonitu).
Za določevanje izločljivega svinca v mineralih in krmah, ki vsebujejo filosilikate (npr. kaolinitna glina), je treba uporabiti postopek mokrega razklopa z dušikovo kislino.
Meja kvantifikacije vseh elementov je pri tej metodi odvisna od matrice vzorca in instrumenta. Za kadmij je običajno treba doseči mejo kvantifikacije 0,05 mg/kg, medtem ko je za svinec običajno treba doseči mejo kvantifikacije 0,5 mg/kg.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-oktober-2017
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SIST EN 15550:2008
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Animal feeding stuffs: Methods of sampling and analysis - Determination of cadmium and
lead by graphite furnace atomic absorption spectrometry (GF-AAS) after pressure
digestion
Futtermittel - Probenahme und Untersuchungsverfahren - Bestimmung von Cadmium
und Blei mittels Graphitrohrofen-Atomabsorptionsspektrometrie (GF-AAS) nach
Druckaufschluss
Aliments des animaux - Méthodes d'échantillonnage et d'analyse - Dosage du cadmium
et du plomb par spectrométrie d'absorption atomique à l'aide d'un four graphite après
minéralisation sous pression
Ta slovenski standard je istoveten z: EN 15550:2017
ICS:
65.120 Krmila Animal feeding stuffs
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EN 15550
EUROPEAN STANDARD
NORME EUROPÉENNE
August 2017
EUROPÄISCHE NORM
ICS 65.120 Supersedes EN 15550:2007
English Version
Animal feeding stuffs: Methods of sampling and analysis -
Determination of cadmium and lead by graphite furnace
atomic absorption spectrometry (GF-AAS) after pressure
digestion
Aliments des animaux - Méthodes d'échantillonnage et Futtermittel - Probenahme und
d'analyse - Dosage du cadmium et du plomb par Untersuchungsverfahren - Bestimmung von Cadmium
spectrométrie d'absorption atomique à l'aide d'un four und Blei mittels Graphitrohrofen-
graphite après minéralisation sous pression Atomabsorptionsspektrometrie (GF-AAS) nach
Druckaufschluss
This European Standard was approved by CEN on 6 February 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: Avenue Marnix 17, B-1000 Brussels
© 2017 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 15550:2017 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 5
5 Reagents . 5
6 Apparatus . 6
7 Sampling . 7
8 Preparation of the test sample . 7
8.1 General . 7
8.2 Animal feeding stuffs which can be ground as such . 7
8.3 Liquid animal feeding stuffs . 8
8.3.1 General . 8
8.3.2 Pre-drying . 8
8.3.3 Freeze-drying . 8
8.4 Mineral matrices . 8
9 Procedure. 8
9.1 Digestion . 8
9.1.1 General . 8
9.1.2 Pressure digestion . 8
9.2 Extractable lead in minerals and feeds containing phyllosilicates (e.g. kaolinite clay)
– extraction with diluted nitric acid . 9
9.3 Calibration . 9
9.4 Determination . 9
9.4.1 General . 9
9.4.2 Determination by AAS graphite furnace – atomic absorption spectrometry . 9
10 Calculation and expression of the result . 10
11 Precision . 10
11.1 Inter-laboratory test . 10
11.2 Repeatability . 10
11.3 Reproducibility . 10
12 Test report . 12
Annex A (informative) Results of the inter-laboratory tests . 13
Annex B (informative) Notes on the detection technique, interferences and quantification,
and pressure digestion . 16
Bibliography . 18
European foreword
This document (EN 15550:2017) 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 February 2018, and conflicting national standards
shall be withdrawn at the latest by February 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 supersedes EN 15550:2007.
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 the elements cadmium and lead in
animal feeding stuffs by graphite furnace atomic absorption spectrometry (GF-AAS) after pressure
digestion.
The method was successfully tested in the range of 0,015 mg/kg to 5,65 mg/kg for Cd and 0,18 mg/kg
to 40,3 mg/kg for lead in 11 animal feeds: 2 complete feeds (pig feed, sheep feed), 2 complementary
feeds (2 mineral feeds), 1 mineral premixture, 4 feed materials (MgO, 2 phosphates, CaCO ) and 2 feed
additives (CuSO , bentonite).
For the determination of extractable lead in minerals and feeds, containing phyllosilicates (e.g. kaolinite
clay) wet digestion with diluted nitric acid should be used.
The method limit of quantification for each element is dependent on the sample matrix as well as the
instrument. For cadmium a limit of quantification of 0,05 mg/kg should normally be obtained while for
lead, a limit of quantification of 0,5 mg/kg should be obtained.
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 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
limit of detection
(LOD)
concentration (mass fraction) derived from the smallest measure that can be detected with reasonable
certainty for a given analytical procedure
Note 1 to entry: xLOD denotes the limit of detection expressed as concentration (mass fraction).
[SOURCE: ISO 11843-1, see [1]]
Note 2 to entry: For analytical systems where the validation range does not include or approach it, the detection
limit does not need to be part of a validation.
[SOURCE: IUPAC 2002, see [2]]
Note 3 to entry: The various conceptual approaches to the subject depend on the estimate of precision at or
near zero concentration (mass fraction) under repeatability or reproducibility conditions.
3.2
limit of quantification
(LOQ)
lowest concentration (mass fraction) determined with satisfactory measurement uncertainty
Note 1 to entry: x denotes the limit of quantification expressed as concentration (mass fraction)
LOQ
[SOURCE: ISO 11843-1, see [1]]
Note 2 to entry: It is useful to state a concentration (mass fraction) below which the analytical method cannot
operate with an acceptable precision. Such precision is arbitrarily defined as relative standard deviation of 10 %.
Note 3 to entry: Usually the limit is set as a fixed multiple (e.g. 3.3) of the detection limit.
Note 4 to entry: Measurements below LOQ are not devoid of information content and are fit for purpose.
[SOURCE: IUPAC 2002, see [2]]
3.3
feed additives
substances that comply with the definition of feed additives given in the Regulation (EC) No 1831/2003
of the European Parliament and of the Council of 22 September 2003 on additives for use in animal
nutrition [3]
3.4
animal feeding stuffs
substances that comply with the definition of animal feeding stuffs given in the Regulation (EC)
No 178/2002 [4]
4 Principle
For the determination of the elements cadmium and lead, a test portion of the sample is digested under
pressure.
The concentration of the elements is determined by graphite furnace atomic absorption spectrometry
(GF-AAS) using external calibration.
The method detection limit for each element is dependent on the sample matrix as well as the
instrument, the type of atomizer and
...
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