EN 15510:2017
(Main)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
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
Relations
Standards Content (Sample)
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
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
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
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
(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
·
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
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
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.
Loading comments...