Animal feeding stuffs: Methods of sampling and analysis - Determination of calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, manganese, cobalt, molybdenum and lead by ICP-AES

This European Standard specifies the inductively coupled plasma atomic emission spectroscopy (ICP-AES) method for the determination of the elements calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, manganese, cobalt, molybdenum and lead.
The elements calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, manganese, cobalt, molybdenum and lead are extracted either in feeds mainly consisting of organic matter after dry ashing and dissolving in hydrochloric acid or in feeds mainly consisting of inorganic matter after wet digestion with hydrochloric acid.
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 was successfully tested for:
-   calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, manganese, cobalt and molybdenum in the following animal feeding stuffs: 2 complete feeds (pig feed, sheep feed), 1 feed material  (phosphate), 1 mineral premixture and 2 complementary feeds (2 mineral feeds),
-   lead in 2 feed materials (phosphate, CaCO3), 2 feed additives (Bentonite, CuSO4), 1 complementary feed (mineral feed)
The method detection limit for each element is dependent on the sample matrix and the instrument. The method is not applicable for the determination of a low concentration of elements. The limit of quantification should be 3 mg/kg or lower.
This method also applies for the determination in products with high element content (>5 %). For this purpose the accuracy of the method has to be checked individually.
NOTE 1   EN 15621 uses the pressure digestion mode, therefore lower results may be obtained with the described method in this standard.

Futtermittel - Probenahme- und Untersuchungsverfahren - Bestimmung von Calcium, Natrium, Phosphor, Magnesium, Kalium, Eisen, Zink, Kupfer, Mangan, Cobalt, Molybdän und Blei mittels ICP-AES

Diese Europäische Norm legt das Verfahren der Atomemissionsspektrometrie mit induktiv gekoppeltem Plasma (ICPAES) zur Bestimmung der Elemente Calcium, Natrium, Phosphor, Magnesium, Kalium, Eisen, Zink, Kupfer, Mangan, Kobalt, Molybdän und Blei fest.
Die Elemente Calcium, Natrium, Phosphor, Magnesium, Kalium, Eisen, Zink, Kupfer, Mangan, Kobalt, Molybdän und Blei werden entweder nach trockenem Veraschen und Auflösen in Salzsäure aus Futtermittel, das größtenteils aus organischer Substanz besteht, oder durch Nassaufschluss mit Salzsäure aus Futtermittel, das größtenteils aus anorganischer Substanz besteht, extrahiert.
Zur Bestimmung von extrahierbarem Blei in Mineralstoffen und Futtermitteln, die Schichtsilikate enthalten (z. B. kaolinitischer Ton), sollte Nassaufschluss mit Salpetersäure verwendet werden.
Das Verfahren wurde erfolgreich geprüft mit:
-   Calcium, Natrium, Phosphor, Magnesium, Kalium, Eisen, Zink, Kupfer, Mangan, Cobalt und Molybdän in den folgenden Futtermitteln: 2 Alleinfuttermittel (Schweine-, Schaffutter), 1 Einzelfuttermittel (Phosphat), 1 Mineralstoffvormischung und 2 Ergänzungsfuttermittel (2 Mineralfutter);
-   Blei in 2 Einzelfuttermitteln (Phosphat, CaCO3), 2 Futtermittel-Zusatzstoffen (Bentonit, CuSO4) und 1 Ergänzungsfuttermittel (Mineralfutter).
Die Nachweisgrenze des Verfahrens hängt bei jedem Element von der Probenmatrix und von dem Gerät ab. Das Verfahren ist nicht zur Bestimmung einer geringen Elementkonzentration anwendbar. Die Bestimmungsgrenze sollte bei 3 mg/kg oder niedriger liegen.
Dieses Verfahren dient ebenfalls zur Bestimmung in Produkten mit hohem Gehalt des zu messenden Elements (> 5 %). Dann muss die Genauigkeit des Verfahrens im Einzelfall geprüft werden.
ANMERKUNG   EN 15621 verwendet die Druckaufschlussmethode, weshalb niedrigere Ergebnisse als nach dem in dieser Norm beschriebenen Verfahren erhalten werden können.

Aliments des animaux - Méthodes d'échantillonnage et d'analyse - Détermination des teneurs en calcium, sodium, phosphore, magnésium, potassium, fer, zinc, cuivre, manganèse, cobalt, molybdène et plomb par ICP-AES

La présente Norme européenne détaille la méthode de spectrométrie d’émission atomique à plasma à couplage inductif (ICP-AES) utilisée pour la détermination de la teneur des éléments calcium, sodium, phosphore, magnésium, potassium, fer, zinc, cuivre, manganèse, cobalt, molybdène et plomb.
Les éléments calcium, sodium, phosphore, magnésium, potassium, fer, zinc, cuivre, manganèse, cobalt, molybdène et plomb sont extraits soit d’aliments composés principalement de matière organique après incinération par voie sèche et dissolution dans de l’acide chlorhydrique, soit d’aliments composés principalement de matière inorganique après minéralisation par voie humide avec de l’acide chlorhydrique.
Pour la détermination de la teneur en plomb extractible des minéraux et aliments contenant des phyllosilicates (par exemple l’argile à kaolinite), il convient d’utiliser la minéralisation par voie humide avec de l’acide nitrique.
La méthode a été soumise à essai avec succès pour :
-   le calcium, le sodium, le phosphore, le magnésium, le potassium, le fer, le zinc, le cuivre, le manganèse, le cobalt et le molybdène contenus dans les aliments pour animaux suivants : 2 aliments complets (aliment pour porc, aliment pour ovin), 1 matière pour aliments (phosphate), 1 pré-mélange minéral et 2 compléments alimentaires (2 aliments minéraux) ;
-   le plomb contenu dans 2 matières pour aliments (phosphate, CaCO3), 2 additifs pour l’alimentation des animaux (bentonite, CuSO4) et 1 complément alimentaire (aliment minéral).
La limite de détection de la méthode pour chacun des éléments est fonction de la matrice de l’échantillon et de l’instrument. Cette méthode ne permet pas la détermination des éléments en faibles concentrations. Il convient que la limite de quantification soit de 3 mg/kg ou moins.
Cette méthode s’applique également à la détermination des éléments dans les produits à forte teneur en éléments (> 5 %). Pour ce faire, l’exactitude de la méthode doit être vérifiée de façon individuelle.
NOTE 1   L’EN 15621 utilise le mode de minéralisation sous pression, c’est pourquoi de faibles teneurs peuvent être obtenues grâce à la méthode décrite dans la présente norme.

Krma: metode vzorčenja in analize - Določevanje kalcija, natrija, fosforja, magnezija, kalija, železa, cinka, bakra, mangana, kobalta, molibdena in svinca z ICP-AES

Ta evropski standard določa metodo atomske emisijske spektroskopije z induktivno sklopljeno plazmo (ICP-AES) za določevanje kalcija, natrija, fosforja, magnezija, kalija, železa, cinka, bakra, mangana, kobalta, molibdena in svinca.
Kalcij, natrij, fosfor, magnezij, kalij, železo, cink, baker, mangan, kobalt, molibden in svinec so izločeni bodisi iz krme, ki je večinoma sestavljena iz organskih snovi, po postopku suhe upepelitve in raztapljanju v klorovodikovi kislini ali iz krme, ki je večinoma sestavljena iz neorganskih snovi, po postopku mokrega razklopa s klorovodikovo kislino.
Za določevanje izločljivega svinca v mineralih in krmah, ki vsebujejo filosilikate (npr. kaolinitna glina), je treba uporabiti postopek mokrega razklopa z dušikovo kislino.
Metoda je bila uspešno preskušena za:
– kalcij, natrij, fosfor, magnezij, kalij, železo, cink, baker, mangan, kobalt in molibden v naslednjih krmah: dveh celovitih krmah (krmi za prašiče, krmi za ovce), eni sestavini krme (fosfat), enem mineralnem premiksu in dveh dopolnilnih krmah (dveh mineralnih krmah),
– svinec v dveh sestavinah krme (fosfatu, CaCO3), dveh dodatkih za krmo (bentonitu, CuSO4), eni dopolnilni krmi (mineralna krma)
Meja zaznavanja vseh elementov je pri tej metodi odvisna od matrice vzorca in instrumenta. Metoda se ne uporablja za določevanje nizkih koncentracij elementov. Meja kvantifikacije mora znašati 3 mg/kg ali manj.
Ta metoda se uporablja tudi za določevanje koncentracije v izdelkih z visoko vsebnostjo elementov (> 5 %). Natančnost metode za ta namen je treba preveriti posebej.
OPOMBA 1: Standard EN 15621 uporablja način razklopa pod tlakom, zato so lahko rezultati, pridobljeni z metodo, opisano v tem standardu, nižji.

General Information

Status
Published
Public Enquiry End Date
19-Dec-2016
Publication Date
06-Sep-2017
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
24-Aug-2017
Due Date
29-Oct-2017
Completion Date
07-Sep-2017

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.,&3$(6Futtermittel - Probenahme- und Untersuchungsverfahren - Bestimmung von Calcium, Natrium, Phosphor, Magnesium, Kalium, Eisen, Zink, Kupfer, Mangan, Cobalt, Molybdän und Blei mittels ICP-AESAliments des animaux - Méthodes d'échantillonnage et d'analyse - Détermination des teneurs en calcium, sodium, phosphore, magnésium, potassium, fer, zinc, cuivre, manganèse, cobalt, molybdène et plomb par ICP-AESAnimal feeding stuffs: Methods of sampling and analysis - Determination of calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, manganese, cobalt, molybdenum and lead by ICP-AES65.120KrmilaAnimal feeding stuffsICS:Ta slovenski standard je istoveten z:EN 15510:2017SIST EN 15510:2017en,fr,de01-oktober-2017SIST EN 15510:2017SLOVENSKI

STANDARDSIST EN 15510:20071DGRPHãþD
SIST EN 15510:2017
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 15510
August
t r s y ICS
x wä s t r Supersedes EN
s w w s rã t r r yEnglish Version

Animal feeding stuffsã Methods of sampling and analysis æ Determination of calciumá sodiumá phosphorusá magnesiumá potassiumá ironá zincá copperá manganeseá cobaltá molybdenum and lead by ICPæAES Aliments des animaux æ Méthodes d 5échantillonnage et d 5analyse æ Détermination des teneurs en calciumá sodiumá phosphoreá magnésiumá potassiumá ferá zincá cuivreá manganèseá cobaltá molybdène et plomb par ICPæAES

Futtermittel æ Probenahmeæ und Untersuchungsverfahren æ Bestimmung von Calciumá Natriumá Phosphorá Magnesiumá Kaliumá Eisená Zinká Kupferá Manganá Cobaltá Molybdän und Blei mittels ICPæAES This European Standard was approved by CEN on

x February
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

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 w w s rã t r s y ESIST EN 15510:2017

EN 15510:2017 (E) 2 Contents Page European foreword ....................................................................................................................................................... 4 1 Scope .................................................................................................................................................................... 5 2 Normative references .................................................................................................................................... 5 3 Terms and definitions ................................................................................................................................... 5 4 Principle ............................................................................................................................................................. 6 5 Reagents ............................................................................................................................................................. 6 6 Apparatus ........................................................................................................................................................... 8 7 Sampling ............................................................................................................................................................. 8 8 Sample preparation ........................................................................................................................................ 9 8.1 General ................................................................................................................................................................ 9 8.2 Animal feeding stuffs, which can be ground as such .......................................................................... 9 8.3 Liquid animal feeding stuffs ........................................................................................................................ 9 8.3.1 General ................................................................................................................................................................ 9 8.3.2 Pre-drying .......................................................................................................................................................... 9 8.3.3 Freeze-drying ................................................................................................................................................... 9 8.4 Mineral matrices ............................................................................................................................................. 9 9 Procedure........................................................................................................................................................... 9 9.1 Digestion ............................................................................................................................................................ 9 9.1.1 Selection of the procedure ........................................................................................................................... 9 9.1.2 Extraction with

HCl ..................................................................................................................................... 10 9.1.3 Dry ashing and extraction with

HCl ...................................................................................................... 10 9.1.4 Wet digestion with HNO3 ........................................................................................................................... 11 9.2 Calibration ...................................................................................................................................................... 11 9.2.1 General ............................................................................................................................................................. 11 9.2.2 External calibration .................................................................................................................................... 11 9.2.3 Standard addition technique ................................................................................................................... 11 9.2.4 Example of calibration with one addition after dry ashing –HCl ................................................ 11 9.2.5 Example of calibration with one addition after wet digestion – 1 % HCl ................................ 12 9.2.6 Example of calibration with one addition after wet digestion with HNO3............................... 12 9.3 Determination ............................................................................................................................................... 12 9.3.1 General ............................................................................................................................................................. 12 9.3.2 Determination by inductively coupled plasma – atomic emission spectrometry ................ 12 10 Calculation and expression of the result ............................................................................................. 13 10.1 General ............................................................................................................................................................. 13 10.2 External calibration .................................................................................................................................... 14 10.3 Standard addition method with only one addition .......................................................................... 14 10.4 Standard addition method with several additions .......................................................................... 14 10.5 Calculation of the element content in the sample ............................................................................ 15 10.6 Example of calculation after standard addition technique with one addition ...................... 16 11 Precision .......................................................................................................................................................... 16 11.1 Inter-laboratory test ................................................................................................................................... 16 11.2 Repeatability .................................................................................................................................................. 16 11.3 Reproducibility ............................................................................................................................................. 16 SIST EN 15510:2017

EN 15510:2017 (E) 3 12 Test report ...................................................................................................................................................... 20 Annex A (informative)

Results of the inter-laboratory test ....................................................................... 21 Annex B (informative)

Notes on the detection technique, interferences and quantification ........ 27 B.1 General ............................................................................................................................................................. 27 B.2 Interferences .................................................................................................................................................. 27 B.2.1 General ............................................................................................................................................................. 27 B.2.2 Spectral interferences ................................................................................................................................. 27 B.2.3 Ionization interferences ............................................................................................................................. 27 B.2.4 Physical interferences ................................................................................................................................ 27 B.3 Quantification and matrix matching...................................................................................................... 27 B.3.1 General ............................................................................................................................................................. 27 B.3.2 Calibration curve .......................................................................................................................................... 28 B.3.3 Matrix matching ............................................................................................................................................ 28 B.3.4 Standard addition ......................................................................................................................................... 28 Bibliography ................................................................................................................................................................. 29

SIST EN 15510:2017

EN 15510:2017 (E) 4 European foreword This document (EN 15510:2017) 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 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 15510:2007. 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. SIST EN 15510:2017

EN 15510:2017 (E) 5 1 Scope This European Standard specifies the inductively coupled plasma atomic emission spectroscopy (ICP-AES) method for the determination of the elements calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, manganese, cobalt, molybdenum and lead. The elements calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, manganese, cobalt, molybdenum and lead are extracted either in feeds mainly consisting of organic matter after dry ashing and dissolving in hydrochloric acid or in feeds mainly consisting of inorganic matter after wet digestion with hydrochloric acid. 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 was successfully tested for: — calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, manganese, cobalt and molybdenum in the following animal feeding stuffs: 2 complete feeds (pig feed, sheep feed), 1 feed material

(phosphate), 1 mineral premixture and 2 complementary feeds (2 mineral feeds), — lead in 2 feed materials (phosphate, CaCO3), 2 feed additives (Bentonite, CuSO4), 1 complementary feed (mineral feed) For elements with a HORRAT value higher than 2 (see Annex A) the method is more applicable as a screening method and not for confirmatory purposes. The method detection limit for each element is dependent on the sample matrix and the instrument. The method is not applicable for the determination of a low concentration of elements. The limit of quantification should be 3 mg/kg or lower. This method also applies for the determination in products with high element content (>5 %). For this purpose the accuracy of the method has to be checked individually. NOTE 1 Results using EN 15550 may be lower than those obtained when applying EN 15621 as pressure digestion is used in EN 15621. 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) smallest measured content from which it is possible to deduce the presence of the analyte with reasonable statistical certainty Note 1 to entry: The limit of detection is numerically equal to three times the standard deviation of the mean of blank determinations (n

s rá were n = number of measures) performed under reproducibility conditions. SIST EN 15510:2017

EN 15510:2017 (E) 6 3.2 limit of quantification (LOQ) lowest content of the analyte that can be measured with reasonable statistical certainty Note 1 to entry: If both trueness and precision are constant over a concentration range around the limit of detection, then the limit of quantification is numerically equal to ten times the standard deviation of the mean of blank determinations (n

s rá were n = number of measures) performed under reproducibility conditions. 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 calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, manganese, cobalt, molybdenum, lead, a test portion of the sample is — dry ashed and dissolved in hydrochloric acid for feeds mainly consisting of organic matter or — wet digested with hydrochloric acid for feeds mainly consisting of inorganic matter. 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 calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, manganese, cobalt, molybdenum and lead is determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) using external calibration or standard addition technique. 5 Reagents Use only reagents of recognized analytical grade, unless otherwise specified. WARNING —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. 5.1 Water, complying with grade 2 as defined in EN ISO 3696. 5.2 Nitric acid, concentrated, not less than 65 % (m/m), having a density of approximately (HNO3) 1,42 g/ml. 5.3 Dilute nitric acid, to be prepared by mixing 1 volume of nitric acid (5.2) with 1 volume of water. 5.4 Nitric acid solution of 5 % (m/v), to be prepared: pipette 160 ml of dilute nitric acid (5.3) into a 1 000 ml volumetric flask (6.7) and fill to the mark with water. 5.5 Nitric acid solution of 2 % (v/v), to be prepared: pipette 20 ml of nitric acid (5.2) into a 1 000 ml volumetric flask (6.7) and fill to the mark with water. SIST EN 15510:2017

EN 15510:2017 (E) 7 5.6 Hydrochloric acid, concentrated, not less than 30 % (mass fraction), having a density of approximately (HCl) 1,15 g/ml. 5.7 Dilute hydrochloric acid, to be prepared by mixing 1 volume of hydrochloric acid (5.6) with 1 volume of water. 5.8 Hydrochloric acid solution of 1 % (m/v), to be prepared: pipette 60 ml of dilute hydrochloric acid (5.7) into a 1 000 ml volumetric flask (6.7) and fill to the mark with water. 5.9 Element stock solutions Ca, Na, P, Mg, K, Fe, Zn, Cu, Mn, Co, Mo, Pb c = 1 000 mg/l. The user should choose a suitable stock solution. Both single-element stock solutions and multi-element stock solutions with adequate specification stating the acid used and the preparation technique are commercially available. It is advisable to use certified stock solutions. Stock solutions are not to be used after the expiry date. Element stock solutions with concentrations different from 1 000 mg/l may also be used. 5.10 Standard solutions 5.10.1 General Depending on the scope, different multi-element standard solutions may be necessary. In general, when combining multi-element standard solutions, their chemical compatibility and the possible hydrolysis of the components shall be regarded. Spectral interferences from other elements in multi-element standard solutions also need to be considered (Annex B, B.2.2). The examples given below also consider the measuring range of various inductively coupled plasma atomic emission spectrometers and the expected concentration of the element in animal feeding stuffs. The multi-element standard solutions are considered to be stable for several months, if stored in the dark. Other combinations of elements at different concentrations can be used, provided that the element stock solutions (5.9) are diluted with the same acid and equal concentration as the acid in the test solution to a range of standards that covers the concentrations of the elements to be determined. 5.10.2 Multi-element standard solution – Ca, Na, P, Mg, K in 1 % HCl c (Ca, Na, P, Mg, K) = 40 mg/l Pipette 40,0 ml of each element stock solution (Ca, Na, P, Mg, K) (5.9) into a 1 000 ml volumetric flask (6.7). Add 60 ml of dilute hydrochloric acid (5.7). Fill to the mark with water and transfer to a suitable storage bottle. 5.10.3 Multi-element standard solution - Fe, Zn, Cu, Mn, Co, Mo in 1 % HCl c (Fe, Zn, Cu, Mn, Co, Mo) = 50 mg/l Pipette 50,0 ml of each element stock solution (Fe, Zn, Cu, Mn, Co, Mo) (5.9) into a 1 000 ml volumetric flask (6.7). Add 60 ml of dilute hydrochloric acid (5.7). Fill to the mark with water and transfer to a suitable storage bottle. SIST EN 15510:2017

EN 15510:2017 (E) 8 5.10.4 Multi-element standard solution – Pb in 5 % HNO3 c (Pb) = 100 mg/l Pipette 100,0 ml of each element stock solution (Pb) (5.9) into a 1 000 ml volumetric flask (6.7). Add 160 ml dilute nitric acid (5.3). Fill to the mark with water and transfer to a suitable storage bottle. 6 Apparatus 6.1 Laboratory grinder 6.1.1 Use laboratory grinders that are equipped such that they do not lead to contamination of the samples. 6.1.2 Laboratory grinder capable of grinding to a particle size of less than or equal to 1 mm, e.g. a knife mill or equivalent. 6.1.3 Laboratory grinder for mineral matrices capable of grinding to a particle size of less than or equal to 0,5 mm, e.g. a ball mill, centrifuge mill or equivalent. 6.1.4 Mortar with pestle, free of contamination. 6.2 Analytical balance, capable of weighing to an accuracy of 1 mg. 6.3 Electric hot plate, with temperature control. 6.4 Ashing crucibles, of platinum, quartz or porcelain. 6.5 Electric muffle-furnace, capable of being maintained at a temperature of 450 °C ± 20 °C. The real temperature in the furnace has to be checked, because this temperature may be substantially different from the adjust temperature. 6.6 Beaker, of capacity 250 ml. 6.7 One-mark volumetric flasks, of capacities 100 ml, 500 ml, 1 000 ml. 6.8 Inductively coupled plasma – Atomic Emission Spectrometer The instrument shall be equipped with a radial plasma as a minimum requirement; an axial plasma is equally acceptable. Background correction shall also be performed when necessary. Settings of the working conditions (e.g. viewing height, gas flows, RF or plasma power, sample uptake rate, integration time, number of measurements) shall be optimized according the manufacturer’s instructions. 6.9 Freeze drying equipment, capable of freeze-drying liquid animal feeding stuffs. 6.10 Oven for pre-drying, capable to hold a temperature of (70±5) °C. 7 Sampling Sampling is not part of the method specified in this Standard. A recommended sampling method is given in EN ISO 6497 [2]. It is important that the laboratory receives a sample that is truly representative and has not been damaged or changed during transport or storage. SIST EN 15510:2017

EN 15510:2017 (E) 9 8 Sample preparation 8.1 General Prepare the test sample in accordance with EN ISO 6498. — Grinding must be carried out in conditions such that the substance is not appreciably heated. — Operation is to be repeated as many times as is necessary and it must be affected as quickly as possible in order to prevent any gain or loss of constituents (water). — Whole ground product is placed in a flask made of e.g. polypropylene, which can be stoppered and stored in such way to prevent any change in composition. — Before any weighing is carried out for the analysis, the whole test sample must be thoroughly mixed for reasons of homogeneity. 8.2 Animal feeding stuffs, which can be ground as such Grind the laboratory sample (usually 500 g), using a grinder (6.1.2) or mortar (6.1.4), until a particle size of 1 mm or less has been reached. 8.3 Liquid animal feeding stuffs 8.3.1 General Liquid feeding stuffs shall be pre-dried according to the procedure described in 8.3.2 or freeze-dried according to the procedure described in 8.3.3. 8.3.2 Pre-drying Pre-dry the laboratory sample at 70 °C ± 5 °C over at least 16 h to reduce the moisture content using an oven (6.10). The mass of the sample before and after the pre-drying is determined using an analytical balance (6.2). Grind the pre-dried sample in accordance with 8.2. 8.3.3 Freeze-drying Freeze-dry the laboratory sample following the instructions of the freeze-drying equipment (6.9). The mass of the sample before and after the freeze-drying is determined using an analytical balance (6.2). Grind the freeze-dried sample in accordance with 8.2. 8.4 Mineral matrices Mineral matrices, except mineral products containing crystalline water, e.g. MgCl2 6H2O, shall be ground using a grinder (6.1.3) or mortar (6.1.4) until a particle size 0,5 mm or less has been reached. Mineral products containing crystalline water should not be ground. 9 Procedure 9.1 Digestion 9.1.1 Selection of the procedure 9.1.1.1 Determination of Ca, Na, P, Mg, K, Fe, Zn, Cu, Mn, Co, Mo, Pb If the test sample is from feeds mainly consisting of inorganic matter or a product potentially containing phosphates, proceed in accordance with 9.1.2. SIST EN 15510:2017

EN 15510:2017 (E) 10 If the test sample is from feeds mainly consisting of organic matter and if it is free from phosphates rendering insoluble products on ashing, proceed in accordance with 9.1.3. If the test sample contains organic substances and phosphates, proceed in accordance with 9.1.2. 9.1.1.2 Determination of extractable Pb For the determination of extractable lead in minerals and feeds, containing phyllosilicates (e.g. kaolinite clay), proceed in accordance with 9.1.4. 9.1.2 Extraction with

HCl Weigh about 1 g of the prepared test sample to the nearest 1 mg into a beaker of 250 ml (6.6). Add 30 ml dilute hydrochloric acid (5.7). Add about 100 ml of water. Cover the beaker (6.6) with a watch-glass and boil for 30 min on a hot plate (6.3). Allow to cool. Transfer the liquid into a 500 ml volumetric flask (6.7), rinsing the beaker and the watch-glass several times with water. Leave to cool, dilute to the mark with water. After homogenizing, filter through a dry folded filter paper into a dry conical flask. Use the first portion of the filtrate to rinse the glass ware and discard that part. If the determination is not carried out immediately, the conical flask with the filtrate shall be stoppered. Carry out a blank determination at the same time as the extraction, with only the reagents and follow the same procedure as for the samples. Proceed in accordance with 9.2. When the expected concentration of the element is lower than 100 mg/kg, proceed as described in 9.1.2, but use 12 ml dilute hydrochloric acid (5.7) and 70 ml of water, and transfer the liquid into a 100 ml volumetric flask (6.7). 9.1.3 Dry ashing and extraction with

HCl Weigh 5 g of the prepared test sample to the nearest 1 mg in an ashing crucible (6.4). Ash in the furnace (6.5), set at a temperature of 450 °C, until white or grey ash is obtained (a small quantity of carbon does not interfere). Transfer the ash to a 250 ml beaker (6.6) with 30 ml of dilute hydrochloric acid (5.7). Add 100 ml of water. Cover the beaker (6.6) with a watch-glass and boil for 30 min on a hot plate (6.3). Allow to cool. Transfer the liquid into a 500 ml volumetric flask (6.7), rinsing the beaker and the watch-glass several times with water. Leave to cool, dilute to the mark with water. After homogenizing, filter through a dry folded filter paper into a dry conical flask. Use the first portion of the filtrate to rinse the glassware and discard that part. If the determination is not carried out immediately, the conical flask with the filtrate shall be stoppered. Carry out a blank determination at the same time as the extraction, with only the reagents and follow the same procedure as for the samples. Proceed in accordance with 9.2. When the expected concentration of the element is lower than 100 mg/kg, proceed as described in 9.1.3, but use 12 ml dilute hydrochloric acid (5.7) and about 70 ml of water, and transfer the liquid into a 100 ml volumetric flask (6.7). SIST EN 15510:2017

EN 15510:2017 (E) 11 9.1.4 Wet digestion with HNO3 Weigh about 2 g of the prepared test sample to the nearest 1 mg into a beaker of 250 ml (6.6). Add 16 ml dilute nitric acid (5.3). Add about 70 ml of water. Cover the beaker (6.6) with a watch-glass and boil for 30 min on a hot plate (6.3). Allow to cool. Transfer the liquid into a 100 ml volumetric flask (6.7), rinsing the beaker and the watch-glass several times with water. Leave to cool, dilute to the ma

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