EN 16206:2012
(Main)Animal feeding stuffs - Determination of arsenic by hydride generation atomic absorption spectrometry (HGAAS) after microwave pressure digestion (digestion with 65 % nitric acid and 30 % hydrogen peroxide)
Animal feeding stuffs - Determination of arsenic by hydride generation atomic absorption spectrometry (HGAAS) after microwave pressure digestion (digestion with 65 % nitric acid and 30 % hydrogen peroxide)
This European Standard specifies a method for the determination of total arsenic in animal feeding stuffs by hydride generation atomic absorption spectrometry (HGAAS) after microwave pressure digestion. The limit of quantification is 0,5 µg/l of the test solution. Using a test portion of 0,5 g, a volume of the test solution of 25 ml and an aliquot of 5 ml for pre-reduction the limit of quantification is 0,125 mg/kg in the feed material.
NOTE For feed materials containing organic arsenic species from compounds of marine origin (i.e. arsenobetaine and tetramethylarsine oxide) a higher digestion temperature of the microwave system up to 300 °C may be necessary in order to enable the hydridisation of these arsenic compounds and in order to determine all different kinds of arsenic species in the corresponding feeding stuffs. Alternatively, the digestion procedure of Annex D can be used if the microwave system does not reach higher temperatures up to 300 °C to ensure complete mineralization for HGAAS determination.
Futtermittel - Bestimmung von Arsen mit Atomabsorptionsspektrometrie-Hydridtechnik (HD-AAS) nach Mikrowellen-Druckaufschluss (Aufschluss mit 65% Salpetersäure und 30% Wasserstoffperoxid)
Diese Europäische Norm legt ein Verfahren zur Bestimmung von Gesamtarsen in Futtermitteln mit der Atomabsorptionsspektrometrie-Hydridtechnik (HD-AAS) (en: Hydride Generation Atomic Absorption Spectrometry, HGAAS) nach Mikrowellen Druckaufschluss fest. Die Bestimmungsgrenze beträgt 0,5 g/l Prüflösung. Bei Verwendung einer Prüfmenge von 0,5 g, eines Volumens der Prüflösung von 25 ml und eines aliquoten Anteils von 5 ml für die Vorreduktion beträgt die Bestimmungsgrenze im Futtermaterial 0,125 mg/kg.
ANMERKUNG Bei Futtermitteln, die organische Arsenspezies aus Verbindungen mariner Herkunft enthalten (z. B. Arsenobetain und Tetramethylarsinoxid), ist möglicherweise eine höhere Aufschlusstemperatur des Mikrowellensystems von bis zu 300 °C erforderlich, um die Hydridbildung dieser Arsenverbindungen zu ermöglichen und alle verschiedenen Arten von Arsenspezies in den entsprechenden Futtermitteln zu bestimmen. Alternativ kann das Aufschlussverfahren in Anhang C angewendet werden, wenn das Mikrowellensystem keine höheren Temperaturen als bis zu 300 °C erreicht, um eine vollständige Mineralisierung für die HD-AAS Bestimmung sicherzustellen.
Aliments pour animaux - Dosage de l'arsenic par spectrométrie d'absorption atomique par génération d'hydrures (SAAGH) après digestion sous pression par micro-ondes (digestion à l'acide nitrique à 65 % et au peroxyde d'hydrogène à 30 %)
La présente Norme européenne spécifie une méthode pour le dosage de l’arsenic total dans les aliments pour
animaux par spectrométrie d’absorption atomique par génération d’hydrures (SAAGH) après digestion sous
pression par micro-ondes. La limite de quantification est égale à 0,5 µg/l de solution d’essai. Avec une prise
d’essai de 0,5 g, un volume de solution d’essai de 25 ml et une partie aliquote de 5 ml pour la préréduction, la
limite de quantification est égale à 0,125 mg/kg dans l'aliment.
NOTE Pour les aliments contenant des espèces d’arsenic organique provenant de composés d’origine marine (par
exemple l’arsénobétaïne et l’oxyde de tétraméthylarsine), une température de digestion plus élevée du système à microondes,
pouvant atteindre 300 °C, peut être nécessaire pour permettre l’hydruration de ces composés de l’arsenic et pour
déterminer toutes les espèces d’arsenic différentes présentes dans les aliments concernés. Il est également possible
d’utiliser le mode opératoire de digestion décrit dans l’Annexe D si le système à micro-ondes ne permet pas d’obtenir des
températures allant jusqu’à 300 °C, assurant une minéralisation complète pour le dosage par SAAGH.
Krma - Določevanje arzena s hidridno atomsko absorpcijsko spektrometrijo (HGAAS) po mikrovalovnem razklopu (razklop s 65 % dušikovo kislino in 30 % vodikovim peroksidom)
Ta evropski standard določa metodo za določevanje celotnega arzena v krmi s hidridno atomsko absorpcijsko spektrometrijo (HGAAS) po mikrovalovnem razklopu. Meja kvantifikacije za preskusno raztopino je 0,5 μg/l. Pri uporabi 0,5 g preskusnega vzorca, 25 ml preskusne raztopine in 5 ml preskusnega deleža za predhodno zmanjšanje se meja kvantifikacije izračuna kot 0,125 mg/kg v krmi.
General Information
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.PHWULMRFuttermittel - Bestimmung von Arsen mit Atomabsorptionsspektrometrie-Hydridtechnik (HD-AAS) nach Mikrowellen-Druckaufschluss (Aufschluss mit 65% Salpetersäure und 30% Wasserstoffperoxid)Aliments pour animaux - Dosage de l'arsenic par spectrométrie d'absorption atomique par génération d'hydrures (SAAGH) après digestion sous pression par micro-ondes (Extraction à l'acide nitrique à 65 % et au peroxyde d'hydrogène à 30 %)Animal feeding stuffs - Determination of arsenic by hydride generation atomic absorption spectrometry (HGAAS) after microwave pressure digestion (digestion with 65 % nitric acid and 30 % hydrogen peroxide)65.120KrmilaAnimal feeding stuffsICS:Ta slovenski standard je istoveten z:EN 16206:2012SIST EN 16206:2012en,fr,de01-april-2012SIST EN 16206:2012SLOVENSKI
STANDARD
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16206
February 2012 ICS 65.120 English Version
Animal feeding stuffs - Determination of arsenic by hydride generation atomic absorption spectrometry (HGAAS) after microwave pressure digestion (digestion with 65 % nitric acid and 30 % hydrogen peroxide)
Aliments pour animaux - Dosage de l'arsenic par spectrométrie d'absorption atomique par génération d'hydrures (SAAGH) après digestion sous pression par micro-ondes (Extraction à l'acide nitrique à 65 % et au peroxyde d'hydrogène à 30 %)
Futtermittel - Bestimmung von Arsen mit Atomabsorptionsspektrometrie-Hydridtechnik (HD-AAS) nach Mikrowellen-Druckaufschluss (Aufschluss mit 65% Salpetersäure und 30% Wasserstoffperoxid) This European Standard was approved by CEN on 30 December 2011.
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, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom.
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Results of the inter-laboratory test . 12Annex B (informative)
Flowchart - Determination of arsenic by hydride generation atomic absorption spectrometry (HGAAS) after microwave pressure digestion (digestion with 65 % nitric acid and 30 % hydrogen peroxide) . 13Annex C (informative)
Alternative digestion procedure with the same digestion efficiency to ensure complete mineralization of all organic and inorganic arsenic species for HGAAS measurement: dry ashing with magnesium oxide and magnesium nitrate as ashing reagents . 15Bibliography . 16 SIST EN 16206:2012
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 6497, Animal feeding stuffs
Sampling (ISO 6497) prEN ISO 6498, Animal feeding stuffs
Guidelines for sample preparation (ISO/DIS 6498) 3 Principle Arsenic is determined in the test solution by hydride generation atomic absorption spectrometry (HGAAS) after microwave pressure digestion and a pre-reduction step. The homogenised feeding stuff test sample is digested by nitric acid and hydrogen peroxide under pressure and high temperatures in a microwave-heated pressure digestion system. Arsenic ions of the test solution are reduced with a potassium iodide/ascorbic acid solution and hydrochloric acid to arsenic (III) and converted to arsenic hydride (AsH3) by sodium borohydride. Arsenic hydride is transferred by a gas stream into a heated measurement cell and decomposed. The absorption at the arsenic line at 193,7 nm corresponds to the amount of arsenic. Since arsenic (III) and arsenic (V) show a different sensitivity with the hydride technique, it is necessary to reduce arsenic (V) to arsenic (III) in order to avoid incorrect measurements.
Other digestion procedures with the same digestion efficiency are possible in order to completely mineralize all arsenic species like organic arsenic species from compounds of marine origin for HGAAS determination (see Annex C). NOTE 1 When using e.g. perchloric acid as alternative digestion procedure to ensure complete mineralisation of all organic and inorganic arsenic species for HGAAS determination you must use NaI/L-ascorbic acid because KI results in precipitation of potassium perchlorate. NOTE 2 Alternatively, inductively-coupled-plasma mass-spectrometry (ICP-MS) for measuring can be used where an incomplete mineralization is not of importance.
WARNING — The use of this 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 standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. SIST EN 16206:2012
NOTE High purity is essential to avoid potential contamination. Therefore, only use reagents available with high purity or perform a digestion by a sub-boiling distillation for nitric acid (4.1). 4.1 Nitric acid, not less than 65 % (mass fraction), of approximately
(HNO3) = 1,4 g/ml. 4.2 Hydrogen peroxide, not less than 30 % (mass fraction), of approximately
(H2O2) ≥≥≥≥ 1,1 g/ml. 4.3 Hydrochloric acid, ≥≥≥≥ 30 % (mass fraction), of approximately
(HCl) ≥≥≥≥ 1,15 g/ml. 4.4 Diluted hydrochloric acid, e.g. about 3 % (mass fraction), used as carrier solution in the flow injection procedure and for dilution of the arsenic stock solution to the 1 mg/l standard solution and furthermore to the calibration solutions. EXAMPLE Dilute approximately 90 ml of hydrochloric acid (4.3) to 1 l with water. 4.5 Sodium borohydride solution, e.g. c = 2 g/l. Dissolve 2 g of sodium hydroxide pellets in water, add 2 g of sodium borohydride and dilute to 1 000 ml with water into 1 000 ml flask (5.3). Prepare a fresh solution daily and, when necessary, filter before use. When the analysis procedure takes longer, it is recommended to cool the sodium borohydride solution, i.e. with ice around the flask, during its use in the HGAAS measurement. NOTE 1 The concentration by mass of the sodium borohydride solution may vary with the system and the instructions of the relevant manufacturer shall therefore be observed.
NOTE 2 Sodium borohydride, stable aq. solution, 4,4 mol/l in 14 mol/l NaOH is also commercially available. WARNING — It is essential to observe the safety instructions for working with sodium borohydride. Sodium borohydride forms hydrogen with acids and this can result in an explosive air/hydrogen mixture. A permanent extraction system shall be provided at the point where measurements are carried out. 4.6 Potassium iodide/ascorbic acid solution. Dissolve 2,5 g of potassium iodide and 2,5 g of L-ascorbic acid in water and dilute to 100 ml. Prepare a fresh solution on the day of the analysis. NOTE The concentrations of the potassium iodide and ascorbic acid may vary slightly with the system and the instructions of the relevant manufacturer shall therefore be observed.
4.7 Arsenic stock solution, c (As) = 1 000 mg/l. Stock solutions are commercially available. It is advisable to use certified stock solutions. Otherwise dissolve 1,320 g of diarsenic trioxide (As2O3) in 25 ml of potassium hydroxide solution (c = 20 g/100 ml), neutralize with 20 % (mass fraction) sulfuric acid with phenolphthalein as indicator and dilute to 1 000 ml with 1 % (mass fraction) sulfuric acid. 4.8 Arsenic standard solution, c (As) = 1 mg/l. Pipette, for example, 100 µl of the stock solution (4.7) into a 100 ml flask (5.3) and fill up with hydrochloric acid (4.4) to reach a concentration of 1 mg/l. SIST EN 16206:2012
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