Fertilizers - Determination of the complexed micro-nutrient content and of the complexed fraction of micro-nutrients

This document specifies a general method for the determination of the micronutrients complexed by complexing agents in fertilizers. The method allows the determination of the total concentration of each complexed micronutrient in complexes, but it does not identify the individual complexing agents.
This procedure concerns EC-fertilizers covered by Regulation (EC) No 2003/2003 [1]. The method is applicable to a mass fraction of the metal complexed of at least 0,07 %, 0,006 % and 0,035 % of Fe, Mn and Zn respectively (see [2]).

Düngemittel - Bestimmung des Gehalts an komplexgebundenen Mikronährstoffionen und der komplexgebundenen Fraktion von Mikronährstoffen

Diese Europäische Norm legt ein allgemeines Verfahren zur Bestimmung der durch Komplexbildner komplex-gebundenen Spurennährstoffe in Düngemitteln fest. Das Verfahren ermöglicht die Bestimmung der Gesamt-konzentration jedes komplexgebundenen Spurennährstoffs nach Subtraktion des Gehalts an chelatisierten Spurennährstoffen, identifiziert jedoch nicht die einzelnen Komplex¬bildner.
Das vorliegende Verfahren gilt für EG Düngemittel, die komplexgebundene Spurennährstoffe enthalten, entsprechend der Verordnung (EG) Nr. 2003/2003 [1]. Das Verfahren gilt für einen Massenanteil an komplexgebundenem Metall von mindestens 0,07 %, 0,006 % bzw. 0,035 % Fe, Mn bzw. Zn (siehe [2]). Eine niedrigere Bestimmungsgrenze ist für Cu und Co nicht festgestellt worden.

Engrais - Détermination des micro-nutriments ironique quels sont complexe manié et de fraction complexe manié des micro-nutriments

La présente norme européenne décrit une méthode générale de dosage, dans des engrais, d’oligo-éléments complexés par des agents complexants. La méthode permet de doser la concentration totale en chaque oligo-élément complexé dans des complexes, après avoir soustrait la teneur en oligo-éléments chélatés, mais ne permet pas d’identifier les différents agents complexants.
Ce mode opératoire concerne les engrais CE qui contiennent des oligo-éléments complexés couverts par le règlement (CE) N°2003/2003. La méthode est applicable à une fraction massique du métal complexé d’au moins 0,07 %, 0,006 % et 0,035 % de Fe, Mn et Zn respectivement (voir [2]). Une limite de quantification plus basse n’a pas été établie pour Cu et Co.

Gnojila - Določevanje kompleksiranih mikrohranil in kompleksiranih frakcij mikrohranil

Ta evropski standard opredeljuje splošno metodo za določevanje mikrohranil, kompleksiranih s kompleksanti, v gnojilih. Metoda omogoča določevanje skupne koncentracije vsakega kompleksiranega mikrohranila v kompleksih po odvzetju vsebnosti kelatnih mikrohranil, vendar ne prepozna posameznih kompleksantov. Ta postopek zadeva gnojila ES, ki vsebujejo kompleksirana mikrohranila, ki jih zajema Uredba (ES) št. 2003/2003. Metoda se uporablja za masni delež kovine, kompleksirane z najmanj 0,07 %, 0,006 % in 0,035 % Fe, Mn in Zn v tem zaporedju (glej [2]). Nižja meja količinskega določanja ni bila vzpostavljena za Cu in Co.

General Information

Status
Published
Public Enquiry End Date
19-Aug-2009
Publication Date
14-Sep-2011
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
08-Sep-2011
Due Date
13-Nov-2011
Completion Date
15-Sep-2011

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.PLNURKUDQLODüngemittel - Bestimmung des Gehalts an komplexgebundenen Mikronährstoffionen und der komplexgebundenen Fraktion von MikronährstoffenEngrais - Détermination des micro-nutriments ironique quels sont complexe manié et de fraction complexe manié des micro-nutrimentsFertilizers - Determination of the complexed micro-nutrient content and of the complexed fraction of micro-nutrients65.080GnojilaFertilizersICS:Ta slovenski standard je istoveten z:EN 15962:2011SIST EN 15962:2011en,fr,de01-oktober-2011SIST EN 15962:2011SLOVENSKI
STANDARD



SIST EN 15962:2011



EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 15962
January 2011 ICS 65.080 English Version
Fertilizers - Determination of the complexed micro-nutrient content and of the complexed fraction of micro-nutrients
Engrais - Dosage de la teneur en oligo-élément complexé et de la fraction complexée des oligo-éléments
Düngemittel - Bestimmung des Gehalts an komplexgebundenen Spurennährstoffionen und der komplexgebundenen Fraktion von Spurennährstoffen This European Standard was approved by CEN on 3 December 2010.
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 and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2011 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15962:2011: ESIST EN 15962:2011



EN 15962:2011 (E) 2 Contents Page Foreword .31Scope .42Normative references .43Principle .44Interferences .45Apparatus .46Reagents .57Preparation of the sample .58Procedure .58.1Preparation of the sample solution .58.2Precipitation .68.3Spectrometric determination .68.4Water-soluble micro-nutrient content determination .69Expression of results .79.1Complexed micro-nutrient content in the fertilizer .79.2Complexed fraction of a micro-nutrient in the fertilizer.710Precision .710.1Inter-laboratory test .710.2Repeatability .810.3Reproducibility .811Test report .8Annex A (informative)
Results of the inter-laboratory test . 10A.1Test samples . 10A.2Inter-laboratory test procedure . 10A.3Results and statistical interpretation. 10Bibliography . 14 SIST EN 15962:2011



EN 15962:2011 (E) 3 Foreword This document (EN 15962:2011) has been prepared by Technical Committee CEN/TC 260 “Fertilizers and liming materials”, the secretariat of which is held by DIN. 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 July 2011, and conflicting national standards shall be withdrawn at the latest by July 2011. 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. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: 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 and the United Kingdom. SIST EN 15962:2011



EN 15962:2011 (E) 4 1 Scope This European Standard specifies a general method for the determination of the micronutrients complexed by complexing agents in fertilizers. The method allows the determination of the total concentration of each complexed micronutrient in complexes after subtraction of the chelated micro-nutrients content, but it does not identify the individual complexing agents. This procedure concerns EC-fertilizers which contain complexed micro-nutrients covered by Regulation (EC) No 2003/2003. The method is applicable to a mass fraction of the metal complexed of at least 0,07 %, 0,006 % and 0,035 % of Fe, Mn and Zn respectively (see [2]). A lower limit of quantification has not been established for Cu and Co. 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 1482-2, Fertilizers and liming materials — Sampling and sample preparation — Part 2: Sample preparation EN ISO 3696:1995, Water for analytical laboratory use — Specification and test methods (ISO 3696:1987) 3 Principle The method is based on the precipitation of the inorganic forms at pH 9. Then the complexed forms of an element remain in solution and are separated from the non complexed forms. The complexed forms are collected and their content determined by spectrometry, as well as the soluble element content. NOTE For additional information see [2] and [3]. 4 Interferences Any substance combining with a micro-nutrient to form a stable soluble compound (chelate or complex) at pH 9, will prevent the precipitation of the metal, and account for a certain degree of complexation. This is the case for chelating agents. If the presence of chelates is suspected the appropriate analytical method should be used (see Bibliography) to identify and quantify the amount of element chelated, that should be subtracted from the amount of the element given by this method in order to obtain the actual amount of element complexed. 5 Apparatus All glassware, filters, and equipment parts coming in contact with samples and solutions, should be appropriate for micro-nutrient analysis, be very clean and free from contamination, especially by the elements Co, Cu, Fe, Mn, and Zn. Usual laboratory equipment, glassware and in particular the following: 5.1 Magnetic stirrer. 5.2 Balance, capable for weighing to an accuracy of 1 mg. 5.3 pH-meter, equipped with a glass electrode; the system shall be calibrated with pH 7 and pH 10 calibration buffers. 5.4 Membrane filters, micro-membrane filters resistant to aqueous solutions, with porosity of 0,45 µm. SIST EN 15962:2011



EN 15962:2011 (E) 5 5.5 Cellulose filters, fast filtration quantitative cellulose filters. 6 Reagents All reagents shall be of recognized analytical grade. 6.1 Water used for the preparation of standard solutions. Water used for the preparation of standard solutions, and sample solutions shall conform to EN ISO 3696:1995, grade 1 and be free of organic contaminants. 6.2 Hydrogen peroxide, H2O2, 30 % to 33 %. 6.3 Sodium hydroxide solution, c(NaOH) = 0,5 mol/l. Carefully dissolve 20,0 g of NaOH in water and dilute to 1 l. This solution is also available commercially. 6.4 Sodium hydroxide solution, c(NaOH) = 0,05 mol/l. Carefully dissolve 2,0 g of NaOH in water and dilute to 1 l. This solution is also available commercially. 6.5 Buffer solution, pH = 7,0. 6.6 Buffer solution, pH = 10,0. 7 Preparation of the sample Sampling is not part of the method specified in this document. A recommended sampling method is given in EN 1482-1. Sample preparation shall be carried out in accordance with EN 1482-2. NOTE For the size reduction of samples with a high amount of complexing agents, it is not recommended to use a high speed laboratory mill. It is more convenient to grind the sample to a particle size less than 1 mm by the use of a mortar and pestle. 8 Procedure 8.1 Preparation of the sample solution Weigh, to the nearest 1 mg, a quantity of the fertilizer between 5 g and 10 g, depending on the declared content of the metal complex, into a 250 ml or 500 ml beaker. Add 200 ml or 400 ml of water. Stir using a magnetic stirrer (5.1) for 1 h. Transfer quantitati
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