EN 17374:2020
(Main)Animal feeding stuffs: Methods of sampling and analysis - Determination of inorganic arsenic in animal feed by anion-exchange HPLC-ICP-MS
Animal feeding stuffs: Methods of sampling and analysis - Determination of inorganic arsenic in animal feed by anion-exchange HPLC-ICP-MS
This document specifies a procedure for the determination of inorganic arsenic in animal feeding stuffs by anion-exchange HPLC-ICP-MS following water bath extraction.
This method was successfully tested in the range of 0,149 mg/kg to 9,69 mg/kg in the following animal feed matrices: rice meal, seaweed meal, fish meal, grass meal, complete feed (marine-based), complete feed (cereal based) and a synthetic solution.
NOTE Mineral feed matrices are not included in the scope of this method. It is good to perform a determination of the total arsenic content in such matrices.
Futtermittel: Probenahme- und Untersuchungsverfahren - Bestimmung von anorganischem Arsen in Futtermittel mittels Anionenaustausch HPLC-ICP-MS
Dieses Dokument legt ein Verfahren zur Bestimmung von anorganischem Arsen in Futtermitteln durch Anionenaustausch-HPLC ICP MS nach Wasserbadextraktion fest.
Dieses Verfahren wurde im Bereich von 0,149 mg/kg bis 9,69 mg/kg für die folgenden Futtermittelmatrices erfolgreich geprüft: Reismehl, Meeresalgenmehl, Fischmehl, Grasmehl, Alleinfuttermittel (auf Basis von Meeres¬produkten), Alleinfuttermittel (auf Getreidebasis) und eine synthetische Lösung.
ANMERKUNG Mineralische Futtermittelmatrices fallen nicht in den Anwendungsbereich dieses Verfahrens. Es wird empfohlen, bei solchen Matrices eine Bestimmung des Gesamtarsengehalts durchzuführen.
Aliments des animaux - Méthodes d’échantillonnage et d’analyse - Détermination de la teneur en arsenic inorganique dans les aliments pour animaux, par CLHP avec échange d’anions et spectrométrie de masse à plasma induit par haute fréquence (ICP-SM)
Le présent document spécifie un mode opératoire pour le dosage de l’arsenic inorganique dans les aliments des animaux par CLHP à échange d’anions ICP-SM après extraction au bain-marie.
Cette méthode a été appliquée avec succès dans la plage allant de 0,149 mg/kg à 9,69 mg/kg dans les matrices d’aliments des animaux suivantes : farine de riz, farine d’algues marines, farine de poisson, farine d’herbes, aliment complet pour animaux (à base de produits de la mer), aliment complet pour animaux (à base de céréales) et une solution de synthèse.
NOTE Les matrices d’aliments minéraux ne sont pas incluses dans le domaine d’application de cette méthode. Il est préférable de réaliser le dosage de l’arsenic total pour ce type de matrices.
Krma: metode vzorčenja in analize - Določevanje anorganskega arzena v krmi z anionsko izmenjevalno HPLC-ICP-MS
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
01-september-2020
Krma: metode vzorčenja in analize - Določevanje anorganskega arzena v krmi z
anionsko izmenjevalno HPLC-ICP-MS
Animal feeding stuffs: Methods of sampling and analysis - Determination of inorganic
arsenic in animal feed by anion-exchange HPLC-ICP-MS
Futtermittel: Probenahme- und Untersuchungsverfahren - Bestimmung von
anorganischem Arsen in Futtermittel mittels Anionenaustausch HPLC-ICP-MS
Aliments des animaux - Méthodes d’échantillonnage et d’analyse - Détermination de la
teneur en arsenic inorganique dans les aliments pour animaux, par CLHP avec échange
d’anions et spectrométrie de masse à plasma induit par haute fréquence (ICP-SM)
Ta slovenski standard je istoveten z: EN 17374:2020
ICS:
65.120 Krmila Animal feeding stuffs
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EN 17374
EUROPEAN STANDARD
NORME EUROPÉENNE
July 2020
EUROPÄISCHE NORM
ICS 65.120
English Version
Animal feeding stuffs: Methods of sampling and analysis -
Determination of inorganic arsenic in animal feed by
anion-exchange HPLC-ICP-MS
Aliments des animaux - Méthodes d'échantillonnage et Futtermittel: Probenahme- und
d'analyse - Détermination de la teneur en arsenic Untersuchungsverfahren - Bestimmung von
inorganique dans les aliments pour animaux, par CLHP anorganischem Arsen in Futtermittel mittels
avec échange d'anions et spectrométrie de masse à Anionenaustausch HPLC-ICP-MS
plasma induit par haute fréquence (ICP-SM)
This European Standard was approved by CEN on 10 May 2020.
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
© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17374:2020 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 . 4
5 Reagents . 4
6 Apparatus and equipment . 6
7 Sampling . 7
8 Procedure. 7
8.1 Sample preparation . 7
8.2 Water bath extraction . 7
8.3 Determination of inorganic arsenic by HPLC-ICP-MS . 8
8.3.1 General . 8
8.3.2 Preparation of apparatus . 8
8.3.3 Calibration . 8
8.3.4 Determination of samples and blank solution . 8
8.3.5 HPLC sequence . 8
8.3.6 Typical HPLC-ICP-MS settings . 9
8.4 Quality control . 9
9 Calculation . 9
9.1 Integration of peaks . 9
9.2 Inorganic arsenic in test solutions . 10
9.3 Calculation of inorganic arsenic in the samples . 10
10 Precision . 10
10.1 Inter-laboratory test . 10
10.2 Repeatability . 10
10.3 Reproducibility . 10
11 Test report . 11
Annex A (informative) Results of the inter-laboratory test . 12
Bibliography . 14
European foreword
This document (EN 17374:2020) 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 January 2021, and conflicting national standards shall
be withdrawn at the latest by January 2021.
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 standardization request given to CEN by the European
Commission and the European Free Trade Association.
WARNING — The method described in this document 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, 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.
1 Scope
This document specifies a procedure for the determination of inorganic arsenic in animal feeding stuffs
by anion-exchange HPLC-ICP-MS following water bath extraction.
This method was successfully tested in the range of 0,149 mg/kg to 9,69 mg/kg in the following animal
feed matrices: rice meal, seaweed meal, fish meal, grass meal, complete feed (marine-based), complete
feed (cereal based) and a synthetic solution.
NOTE Mineral feed matrices are not included in the scope of this method. It is good to perform a
determination of the total arsenic content in such matrices.
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).
EN ISO 3696:1995, Water for analytical laboratory use — Specification and test methods (ISO 3696:1987)
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 https://www.iso.org/obp
4 Principle
This document describes a method for the determination of inorganic arsenic in animal feeding stuffs.
Inorganic arsenic consists of arsenite, As(III) and arsenate, As(V). A representative test portion of the
sample is treated with a diluted nitric acid and hydrogen peroxide solution in a heated water bath.
Hereby the arsenic species are extracted into solution and As(III) is oxidized to As(V). The inorganic
arsenic is selectively separated from other arsenic compounds using anion exchange HPLC (High
Performance Liquid Chromatography) coupled online to the element-specific detector ICP-MS
(Inductively Coupled Plasma Mass Spectrometry) for the determination of the mass fraction of
inorganic arsenic. External calibration with solvent matrix-matched standards is used for quantification
of the amount of inorganic arsenic.
5 Reagents
Use only reagents of recognized analytical grade and water conforming to grade 1 of EN ISO 3696:1995.
5.1 General
The concentration of arsenic species in the reagents and water used shall be low enough to not affect
the results of the determination. Reagents should be of minimum p.a. quality where possible. Special
facilities should be used in order to avoid contamination during the steps of preparation and
measurement (e.g. laminar flow benches or comparable clean facilities).
When using a method of high sensitivity like ICP-MS, the control of the blank levels of water, acid and
other reagents is very important. Generally ultra-pure water complying with grade 1 of
EN ISO 3696:1995 (i.e. electrical conductivity below 0,1 μS/cm at 25 °C) and acid of high purity, e.g.
cleaned by sub-boiling distillation, are recommended.
5.2 Nitric acid HNO concentrated, ≥ 65 % (mass fraction), mass concentration of approximately
ρ(HNO ) = 1,4 g/ml.
Use only nitric acid available with high purity or perform a clean-up by a sub-boiling distillation in
order to avoid potential contamination.
5.3 Hydrogen peroxide, H O not less than 30 % (mass fraction).
2 2
High purity is essential to avoid potential contamination. Commercially available hydrogen peroxide for
analysis should be tested for contamination of arsenic prior to use.
5.4 Extraction solution 1, 0,1 mol/l HNO in a volume fraction of 3 % H O .
3 2 2
Pour 800 ml of water and then 6,5 ml of nitric acid (5.2) and thereafter 100 ml of hydrogen peroxide
(5.3) into a 1 000 ml volumetric flask. Fill it up to the mark with water. This solution should be prepared
on the same day of use.
It is recommended that the total volume needed for the analysis is estimated and only this amount is
produced.
5.5 Extraction solution 2, 0,2 mol/l HNO in 6 % H O .
3 2 2
Pour 70 ml of water, 1,3 ml of nitric acid (5.2) and 20 ml of hydrogen peroxide (5.3) into a 100 ml
volumetric flask. Fill it up to the mark at 100 ml with water. This solution should be prepared on the
same day of use.
It is recommended that the total volume needed for the analysis is estimated and only this amount is
produced.
5.6 Ammonium carbonate, (NH ) CO , mass fraction w ≥ 99,999 %, for production of mobile phase
4 2 3
solution.
5.7 Aqueous ammonia, (NH (aq)) w ≥ 25 %, for adjustment of pH in the mobile phase.
5.8 Methanol, (CH OH), HPLC grade, for production of mobile phase.
5.9 Mobile phase, e.g. 50 mmol/l ammonium carbonate in 3 % methanol at pH 10,3.
Dissolve e.g. 4,80 g of ammon
...
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