CEN/TS 15621:2007
(Main)Animal feeding stuffs - Determination of calcium, sodium, phosphorus, magnesium, potassium, sulphur, iron, zinc, copper, manganese, cobalt and molybdenum after pressure digestion by ICP-AES
Animal feeding stuffs - Determination of calcium, sodium, phosphorus, magnesium, potassium, sulphur, iron, zinc, copper, manganese, cobalt and molybdenum after pressure digestion by ICP-AES
This Technical Specification specifies a method for the determination of the minerals calcium, sodium, phosphorus, magnesium, potassium and sulphur and the elements iron, zinc, copper, manganese, cobalt, molybdenum in animal feeding stuffs by inductively coupled plasma atomic emission spectrometry (ICP-AES) after pressure digestion.
The method limit of quantification for each element is dependent on the sample matrix as well as of the instrument. The method is not applicable for determination of low concentrations of elements. A limit of quantification of 1 mg/kg should normally be obtained.
Futtermittel - Bestimmung von Calcium, Natrium, Phosphor, Magnesium, Kalium, Schwefel, Eisen, Zink, Kupfer, Mangan, Kobalt und Molybdän nach Druckaufschluss mittels ICP-AES
Aliments pour animaux - Détermination du calcium, du sodium, du phosphore, du magnésium, du potassium, du soufre, du fer, du zinc, du cuivre, du manganèse, du cobalt et du molybdène après digestion sous pression par spectrométrie d'émission atomique à plasma à couplage inductif (spectrométrie ICP-AES)
La présente Spécification Technique spécifie une méthode de détermination de la teneur en minéraux (calcium, sodium, phosphore, magnésium, potassium, souffre) et de la teneur en éléments (fer, zinc, cuivre, manganèse, cobalt, molybdène) présents dans les aliments pour animaux par spectrométrie d'émission atomique à plasma à couplage inductif (spectrométrie ICP AES) après digestion sous pression.
La limite de quantification 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 de parvenir à une limite de quantification de 1 mg/kg, dans des conditions normales d'essai.
Krma - Določevanje kalcija, natrija, fosforja, magnezija, kalija, žvepla, železa, cinka, bakra, mangana, kobalta in molibdena po razklopu pod tlakom z ICP-AES
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-november-2007
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EDNUDPDQJDQDNREDOWDDQGPROLEGHQDSRUD]NORSXSRGWODNRP],&3$(6
Animal feeding stuffs - Determination of calcium, sodium, phosphorus, magnesium,
potassium, sulphur, iron, zinc, copper, manganese, cobalt and molybdenum after
pressure digestion by ICP-AES
Futtermittel - Bestimmung von Calcium, Natrium, Phosphor, Magnesium, Kalium,
Schwefel, Eisen, Zink, Kupfer, Mangan, Kobalt und Molybdän nach Druckaufschluss
mittels ICP-AES
Aliments pour animaux - Détermination du calcium, du sodium, du phosphore, du
magnésium, du potassium, du soufre, du fer, du zinc, du cuivre, du manganese, du
cobalt et du molybdene apres digestion sous pression par spectrométrie d'émission
atomique a plasma couplage inductif (spectrométrie ICP-AES)
Ta slovenski standard je istoveten z: CEN/TS 15621:2007
ICS:
65.120 Krmila Animal feeding stuffs
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
TECHNICAL SPECIFICATION
CEN/TS 15621
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
August 2007
ICS 65.120
English Version
Animal feeding stuffs - Determination of calcium, sodium,
phosphorus, magnesium, potassium, sulphur, iron, zinc, copper,
manganese, cobalt and molybdenum after pressure digestion by
ICP-AES
Aliments pour animaux - Détermination du calcium, du Futtermittel - Bestimmung von Calcium, Natrium,
sodium, du phosphore, du magnésium, du potassium, du Phosphor, Magnesium, Kalium, Schwefel, Eisen, Zink,
soufre, du fer, du zinc, du cuivre, du manganèse, du cobalt Kupfer, Mangan, Kobalt und Molybdän nach
et du molybdène après digestion sous pression par Druckaufschluss mittels ICP-AES
spectrométrie d'émission atomique à plasma couplage
inductif (spectrométrie ICP-AES)
This Technical Specification (CEN/TS) was approved by CEN on 9 June 2007 for provisional application.
The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to submit their
comments, particularly on the question whether the CEN/TS can be converted into a European Standard.
CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS available
promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the CEN/TS)
until the final decision about the possible conversion of the CEN/TS into an EN is reached.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, 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 and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36 B-1050 Brussels
© 2007 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 15621:2007: E
worldwide for CEN national Members.
Contents Page
1 Scope .4
2 Normative references .4
3 Terms and definitions .4
4 Principle.5
5 Reagents.5
6 Apparatus .6
7 Sampling.6
8 Preparation of the test sample .7
9 Procedure .7
10 Calculation and expression of the result .9
11 Precision.12
12 Test report .15
Annex A (informative) Results of the interlaboratory tests.16
Annex B (informative) Notes on the detection technique, interferences and quantification,
pressure digestion.20
Foreword
This document (CEN/TS 15621:2007) 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.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to announce this Technical Specification: Austria, Belgium, Bulgaria, 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 and United Kingdom.
1 Scope
This Technical Specification specifies a method for the determination of the minerals calcium, sodium,
phosphorus, magnesium, potassium and sulphur and the elements iron, zinc, copper, manganese, cobalt,
molybdenum in animal feeding stuffs by inductively coupled plasma atomic emission spectrometry (ICP-AES)
after pressure digestion.
The method limit of quantification for each element is dependent on the sample matrix as well as of the
instrument. The method is not applicable for determination of low concentrations of elements. A limit of
quantification of 1 mg/kg should normally be obtained.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.
EN 13805: 2002, Foodstuffs – Determination of trace elements – Pressure digestion.
EN ISO 3696:1995, Water for analytical laboratory use – Specification and test methods (ISO 3696:1987).
ISO 6498:1998, Animal feeding stuffs – Preparation of test samples.
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 The limit of detection is numerically equal to three times the standard deviation of the mean of blank
determinations (n ≥ 10, were n = number of measures) performed under reproducibility conditions.
3.2
limit of quantification (LOQ)
lowest content of the analyte which can be measured with reasonable statistical certainty
NOTE 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 ≥ 10,
were n = number of measures) performed under reproducibility conditions.
3.3
feed additives
substances are feed additives when they comply with the definition of feed additives given in regulation EU
1831/2003
3.4
animal feeding stuffs
substances are animal feeding stuffs when they comply with the definition of animal feeding stuffs given in
regulation EU 178/2002
4 Principle
For the determination of calcium, sodium, phosphorus, magnesium, potassium, sulphur, iron, zinc, copper,
manganese, cobalt and molybdenum, a test portion of the sample is digested under pressure.
The concentration of the elements is determined by inductively coupled plasma atomic emission spectrometry
(ICP-AES) using external calibration or standard addition technique.
WARNING – The use of this Technical Specification can involve hazardous materials, operations and equipment.
This Specification does not purport to address all the safety problems associated with its use. It is the
responsibility of the user of this Technical Specification to establish appropriate safety and health practices and
determine the applicability of regulatory limitations prior to use.
5 Reagents
Use only reagents of recognized analytical grade, unless otherwise specified.
5.1 Water, complying with grade 2 as defined in EN ISO 3696.
5.2 Nitric acid, concentrated, not less than 65 % (mass fraction), c(HNO ) = 14,4 mol/l, having a
density of approximately ρ (HNO ) 1,42 g/ml.
5.3 Nitric acid solution of 2 % (v/v), to be prepared: pipette 20 ml nitric acid (5.2) in a 1000 ml
volumetric flask (6.4) and fill to the mark with water.
5.4 Hydrogen peroxide, not less than 30 % (mass fraction).
5.5 Element stock solutions
Ca, Na, P, Mg, K, S, Fe, Zn, Cu, Mn, Co, Mo
c = 1000 mg/l.
The user shall 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.
NOTE Element stock solutions with concentrations different from 1000 mg/l may be used as well.
5.6 Standard solutions
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 present in multi-element standards
also need to be considered.
Various combinations of elements at different concentrations can be used, provided that the element stock
solutions (5.5) 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.
The multi-element standard solutions are considered to be stable for several months, if stored in the dark.
6 Apparatus
Usual laboratory apparatus and, in particular, the following.
NOTE For the determination of sodium in low concentrations it is advisable not to use glassware since glassware can
be a source of sodium contamination.
6.1 Laboratory grinder
6.1.1 Laboratory grinder capable of grinding to a particle size of less than or equal to 1 mm, e.g. a knife mill
or equivalent.
6.1.2 Laboratory grinder capable of grinding to a particle size of less than or equal to 0,1 mm, e.g. a ball mill
or equivalent.
6.1.3 Mortar with pestle, free of contamination.
NOTE It should be checked that the mill used does not influence the concentration of elements in the sample (e.g.
adsorption, contamination) which have to be analysed.
6.2 Analytical balance, capable of weighing to an accuracy of 1 mg.
6.3 Pressure digestion apparatus, commercially available.
The apparatus shall be tested for safety pressure vessels made of acid-resistant materials and having holders
for the sample of acid-resistant material with low level of contamination by elements to be determined.
Apparatus is available which uses a high-pressure incinerator with or without ambient autoclave pressure.
Instead of polytetrafluoroethylene (PTFE) holders, it is better to use graduated quartz holders, perfluoro
ethylene propylene (FEP) holders or perfluoro alkoxy (PFA) holders. Quartz is advisable to be used for
decomposition temperatures above 230 °C.
6.4 One-mark volumetric flasks, of capacity 1000 ml.
6.5 Inductively coupled plasma – Atomic Emission Spectrometer
The instrument shall be equipped with radial plasma as a minimum requirement; 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 replicates, …) shall be optimised according the manufacturer’s instructions.
6.6 Freeze drying equipment, capable of freeze-drying liquid animal feeding stuffs.
7 Sampling
Sampling is not part of the method specified in this International Standard. A recommended sampling method
is given in EN-ISO 6497[1].
It is important that the laboratory receives a sample which is truly representative and has not been damaged
or changed during transport or storage.
8 Preparation of the test sample
8.1 General
Prepare the test sample in accordance with ISO 6498.
The grinding must be done in conditions such that the substance is not appreciably heated and that no
contamination takes place by the grinding tools.
The 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).
The 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. Since a maximum of 0,5 g of sample is used for the digestion it is of the utmost
importance to have a homogeneous sample in order to take a representative sub sample.
8.2 Animal feeding stuffs which can be ground as
...
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