Animal feeding stuffs: Methods of sampling and analysis - Determination of iodine in animal feed by ICP-MS

This European standard specifies a method for the determination of iodine in animal feeding stuffs by inductively coupled plasma mass spectrometry (ICP-MS) following extraction with an alkaline solution.
This method was successfully tested in the range of 0,70 to 631 mg/kg in following animal feeds: seaweed meal, mineral premixture, fish meal, plant based ingredient, marine based compound feed and a synthetic iodine solution.

Futtermittel - Probenahme- und Untersuchungs-verfahren - Bestimmung von Iod in Futtermitteln mittels Anionenaustausch ICP-MS

Diese Europäische Norm legt ein Verfahren zur Bestimmung von Iod in Futtermitteln mit der Massenspektrometrie und induktiv gekoppeltem Plasma (ICP-MS) nach dessen Extraktion mit einer alkalischen Lösung fest.
Dieses Verfahren wurde im Bereich von 0,70 mg/kg bis 631 mg/kg in folgenden Futtermitteln angewendet: Seealgenmehl, Mineralstoffvormischung, Fischmehl, pflanzlicher Wirkstoff, Mischfutter aus Meerestieren und eine synthetische Iodlösung.

Aliments pour animaux - Méthodes d’échantillonnage et d’analyse - Dosage de l’iode dans les aliments pour animaux par spectrométrie de masse à plasma induit par haute fréquence (ICP-MS)

La présente Norme européenne spécifie une méthode de dosage de l’iode dans les aliments pour animaux par spectrométrie de masse à plasma induit par haute fréquence (ICP-MS) après extraction avec une solution alcaline.
Cette méthode a été soumise à essai avec succès dans la plage de 0,70 mg/kg à 631 mg/kg avec les aliments pour animaux suivants : farine d’algue, prémélange minéral, farine de poisson, ingrédient à base de plante, aliments composés d’origine marine et une solution d’iode synthétique.

Krma: metode vzorčenja in analize - Določevanje joda v krmi z masno spektrometrijo z induktivno sklopljeno plazmo (ICP-MS)

Ta evropski standard določa metodo za določevanje joda v krmi z masno spektrometrijo z induktivno sklopljeno plazmo (ICP-MS) po ekstrakciji z alkalno raztopino.
Ta metoda je bila uspešno preskušena v razponu od 0,70 do 631 mg/kg pri naslednjih vrstah krme: moka iz morskih alg, mineralni premiks, ribja moka, rastlinska sestavina, morska krmna mešanica in sintetična raztopina joda.

General Information

Status
Published
Public Enquiry End Date
19-Dec-2016
Publication Date
12-Oct-2017
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
05-Oct-2017
Due Date
10-Dec-2017
Completion Date
13-Oct-2017

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Standards Content (Sample)

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.QRFuttermittel - Probenahme- und Untersuchungs-verfahren - Bestimmung von Iod in Futtermitteln mittels Anionenaustausch ICP-MSAliments pour animaux - Méthodes d’échantillonnage et d’analyse - Dosage de l’iode dans les aliments pour animaux par spectrométrie de masse à plasma induit par haute fréquence (ICP-MS)Animal feeding stuffs: Methods of sampling and analysis - Determination of iodine in animal feed by ICP-MS65.120KrmilaAnimal feeding stuffsICS:Ta slovenski standard je istoveten z:EN 17050:2017SIST EN 17050:2017en,fr,de01-november-2017SIST EN 17050:2017SLOVENSKI
STANDARD



SIST EN 17050:2017



EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 17050
September
t r s y ICS
x wä s t r English Version
Animal feeding stuffsã Methods of sampling and analysis æ Determination of iodine in animal feed by ICPæMS Aliments pour animaux æ Méthodes d 5échantillonnage et d 5analyse æ Dosage de l 5iode dans les aliments pour animaux par spectrométrie de masse à plasma induit
Futtermittel æ Probenahmeæ und Untersuchungsæverfahren æ Bestimmung von Iod in Futtermitteln mittels Anionenaustausch ICPæMS This European Standard was approved by CEN on
t z June
t r s yä
egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä
translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä
CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Serbiaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey and United Kingdomä
EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels
9
t r s y CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s y r w rã t r s y ESIST EN 17050:2017



EN 17050:2017 (E) 2 Contents Page European foreword . 4 1 Scope . 5 2 Normative references . 5 3 Principle . 5 4 Reagents . 5 4.1 General . 5 4.2 Tetra methyl ammonium hydroxide (TMAH (CH3)4N+OH «) solution . 5 4.3 Diluted tetra methyl ammonium hydroxide (TMAH) solution . 6 4.4 Stock solutions . 6 4.4.1 General . 6 4.4.2 Iodine stock solution (KIO3 = 1 000 mg/l, purity: mass fraction w > 99,5 % . 6 4.4.3
= 1 000 mg/l . 6 4.5 Standard solutions . 6 4.5.1
= 10 mg/l . 6 4.5.2 Tellurium standard solution (internal standard) . 6 4.6 Iodine calibration solutions . 6 4.6.1 General . 6 4.6.2 Calibration solution 1 -
= 5 µg/l. 7 4.6.3 Calibration solution 2 -
= 20 µg/l . 7 4.6.4 Calibration solution 3 -
= 50 µg/l . 7 4.7 Zero member compensation solution. 7 5 Apparatus and equipment . 7 5.1 General . 7 5.2 Containers . 7 5.3 Plastic syringes . 7 5.4 Membrane filters . 7 5.5 Ultracentrifuge . 8 5.6 Drying oven . 8 5.7 Inductively coupled plasma mass spectrometer (ICP-MS). 8 5.8 Tubes . 8 6 Sampling . 8 6.1 General . 8 6.2 Sampling procedure . 8 7 Procedure. 8 7.1 Sample preparation . 8 7.2 Iodine extraction . 8 7.3 Preparation of sample and blank solutions . 9 7.4 Determination of iodine by ICP-MS . 9 7.4.1 General . 9 7.4.2 Preparation of apparatus . 9 7.4.3 Calibration . 9 7.4.4 Determination . 10 8 Calculation . 10 SIST EN 17050:2017



EN 17050:2017 (E) 3 9 Limit of quantification (LOQ) . 10 10 Precision . 10 10.1 Inter-laboratory test . 10 10.2 Repeatability . 10 10.3 Reproducibility . 11 11 Test report . 11 Annex A (informative)
Results of the inter-laboratory test . 12 Bibliography . 15
SIST EN 17050:2017



EN 17050:2017 (E) 4 European foreword This document (EN 17050:2017) has been prepared by Technical Committee CEN/TC 327 “Animal feeding stuffs”, 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 March 2018, and conflicting national standards shall be withdrawn at the latest by March 2018. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN [and/or CENELEC] 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, and supports essential requirements of EU Directive(s). 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. SIST EN 17050:2017



EN 17050:2017 (E) 5 1 Scope This European standard specifies a method for the determination of iodine in animal feeding stuffs by inductively coupled plasma mass spectrometry (ICP-MS) following extraction with an alkaline solution. This method was successfully tested in the range of 0,70 to 631 mg/kg in following animal feeds: seaweed meal, mineral premixture, fish meal, plant based ingredient, marine based compound feed and a synthetic iodine solution. 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 15111, Foodstuffs - Determination of trace elements - Determination of iodine by ICP-MS (inductively coupled plasma mass spectrometry) EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696) EN ISO 6497, Animal feeding stuffs - Sampling (ISO 6497) EN ISO 6498, Animal feeding stuffs - Guidelines for sample preparation (ISO 6498) 3 Principle This standard describes a method for the determination of iodine in animal feeding stuffs. A representative test portion of the sample is treated with a strong alkaline solution of tetra methyl ammonium hydroxide (TMAH) and incubated at 90°C for three hours. Hereby iodine is extracted into solution and is determined by use of inductively coupled plasma mass spectrometry (ICP-MS). The method principles are the same as used in EN 15111. 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. 4 Reagents Use only reagents of recognized analytical grade and water conforming to grade 2 of EN ISO 3696. 4.1 General The concentration of iodine in the reagents and water used shall be low enough not to affect the results of the determination. NOTE Different qualities of tetra methyl ammonium hydroxide (TMAH) are available and it is important to check that the iodine content is sufficiently low and does not affect the analysis. 4.2 Tetra methyl ammonium hydroxide (TMAH (CH3)4N+OH «) solution
= 250 g/l, (mass fraction w = 25 %), suitable for trace analysis with an iodine content of less than 1 µg/l. SIST EN 17050:2017



EN 17050:2017 (E) 6 4.3 Diluted tetra methyl ammonium hydroxide (TMAH) solution Dilute TMAH solution for preparing the zero member compensation and calibration solutions with a concentration to suit that of the sample solution (see 7.3). Prepare a 0,5 % TMAH solution by diluting e.g. 1,0 ml of TMAH solution (4.2) to 50 ml with water. 4.4 Stock solutions 4.4.1 General Commercially available standard stock solutions of iodine and tellurium are recommended. As an alternative the solutions described below may be used. 4.4.2 Iodine stock solution (KIO3 = 1 000 mg/l, purity: mass fraction w > 99,5 % Dissolve 1,686 4 g of potassium iodate in water and dilute to 1 000 ml with water. 4.4.3
= 1 000 mg/l Dissolve 1,250 8 g of tellurium dioxide (TeO2) in 4 mol/l hydrochloric acid (HCl) and dilute to 1 000 ml with water. 4.5 Standard solutions 4.5.1
= 10 mg/l Pipette 1 ml of the iodine stock solution (4.4.2) into a 100 ml volumetric flask and dilute to the mark with water. This solution is stable for about four weeks and is used to prepare the calibration solutions in 4.6. 4.5.2 Tellurium standard solution (internal standard) Prepare e.g. a 10 mg/l standard tellurium solution by pipetting 1 ml of the tellurium stock solution (4.4.3) into a 100 ml volumetric f
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