Animal feeding stuffs: Methods of sampling and analysis - Determination of inorganic arsenic in animal feed by anion-exchange HPLC-ICP-MS

This method procedure describes a procedure for the determination of inorganic arsenic in animal feeding stuffs by anion-exchange HPLC-ICP-MS following water bath extraction.

Futtermittel: Probenahme- und Untersuchungsverfahren - Bestimmung von anorganischem Arsen in Futtermittel mittels Anionenaustausch HPLC-ICP-MS

Diese Norm beschreibt ein Verfahren zur Bestimmung von anorganischem Arsen in Futtermitteln durch Anionenaustausch-HPLC ICP MS nach Wasserbadextraktion.
Dieses Verfahren wurde im Bereich von 0,149 mg/kg bis 9,69 mg/kg für die folgenden Futtermittelmatrices erfolgreich geprüft: Reismehl, Seealgenmehl, Fischmehl, Grasmehl, Alleinfuttermittel (auf Basis von Meeresprodukten), Alleinfuttermittel (auf Getreidebasis) und eine synthetische Lösung.
ANMERKUNG   Mineralische Futtermittelmatrices fallen nicht in den Anwendungsbereich dieses Verfahrens, da bei solchen Matrices die Bestimmung des Gesamtarsengehalts besser geeignet ist.

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)

La présente méthode décrit 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, car le dosage de l’arsenic total est plus approprié pour ce type de matrices.

Krma: metode vzorčenja in analize - Določevanje anorganskega arzena v krmi z anionsko izmenjevalno HPLC-ICP-MS

General Information

Status
Published
Public Enquiry End Date
09-Jun-2019
Publication Date
15-Jul-2020
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
14-Jul-2020
Due Date
18-Sep-2020
Completion Date
16-Jul-2020

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SLOVENSKI STANDARD
SIST EN 17374:2020
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
SIST EN 17374:2020 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN 17374:2020
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SIST EN 17374:2020
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.
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SIST EN 17374:2020
EN 17374:2020 (E)
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

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SIST EN 17374:2020
EN 17374:2020 (E)
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.
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SIST EN 17374:2020
EN 17374:2020 (E)
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.
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SIST EN 17374:2020
EN 17374:2020 (E)

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 ammonium carbonate (5.6) in approximately 800 ml of water. Adjust the pH to

10,3 with aqueous ammonia (5.7) and add 30 ml of methanol (5.8). Then fill up to 1 000 ml with water.

Filter the mobile phase solution through a 0,45 µm filter prior to use (6 .7).

The optimal concentration of ammonium carbonate in the mobile phase depends on the

analytical column used (e.g. brand, particle size and dimensions). The appropriate concentration

of ammonium carbonate is in the discretion of the analyst and should fulfil the criteria for sufficient

resolution of the arsenate peak as stated in 6.10.

Methanol is added to the mobile phase in order to enhance the signal intensity for arsenic (carbon

enhancement effect [1]). The concentration of methanol for maximum signals depends on the

instrument used and should be identified by the analyst.
5.10 Diarsenic trioxide, w(As O ) ≥ 99,5 %, optional.
2 3
5.11 Potassium hydroxide solution, ρ(KOH) = 20 g/100 ml, optional.
SO ) = 20 % and w(H SO ) = 1 %, optional.
5.12 Sulfuric acid solutions, w(H2 4 2 4
5.13 Phenolphthalein, optional.
5.14 Standard solutions, with an arsenic mass concentration of 1 000 mg/l.

The use of commercial standards of arsenic, As(III) and/or As(V), with a mass concentration of

1 000 mg/l is recommended.
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SIST EN 17374:2020
EN 17374:2020 (E)

Otherwise proceed as follows: Dissolve e.g. 1,320 g of diarsenic trioxide (5.10) in 2

...

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