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STANDARDSIST-TS CEN/TS 15452:20081DGRPHãþD
SIST EN 15452:2009
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 15452July 2008ICS 65.080Supersedes CEN/TS 15452:2006
English VersionFertilizers - Determination of chelating agents - Determination ofiron chelated by o,p-EDDHA by reversed phase HPLCEngrais - Dosage des agents chélatants - Dosage du ferchélaté par o,p-EDDHA par chromatographie liquide àhaute performance à polarité de phase inverséeDüngemittel - Bestimmung von Chelatbildnern -Bestimmung von Eisen-chelatisiertem o,p-EDDHA mitUmkehrphasen HPLCThis European Standard was approved by CEN on 30 May 2008.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the CEN 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 translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.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 STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2008 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15452:2008: ESIST EN 15452:2009
EN 15452:2008 (E) 2 Contents Page Foreword.3 1 Scope.4 2 Normative references.4 3 Principle.4 4 Interferences.4 5 Reagents.4 6 Apparatus.5 7 Sampling and sample preparation.6 8 Procedure.6 9 Expression of results.8 10 Precision.8 11 Test report.9 Annex A (informative)
Typical chromatogram.10 Annex B (informative)
Statistical results of the inter-laboratory test.11 Annex C (informative)
Complete names of chelating agents.12 Bibliography.13
SIST EN 15452:2009
EN 15452:2008 (E) 3 Foreword This document (EN 15452:2008) 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 January 2009, and conflicting national standards shall be withdrawn at the latest by January 2009. 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 supersedes CEN/TS 15452:2006. 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, 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 15452:2009
EN 15452:2008 (E) 4
1 Scope This European Standard specifies a method for the chromatographic determination of the amount of iron chelated by each of the individual isomers of the chelating agent ortho-para EDDHA (o,p-EDDHA) in fertilizers. The method allows the identification of this chelating agent and the determination of the water soluble fraction of iron chelated by this chelating agent. The method is not applicable for the determination of the amount of free chelating agent. NOTE 1 This method has been shown to be also suitable for the determination of the amount of iron chelated by each of the individual isomers of the chelating agent ortho-ortho EDDHA (o,o-EDDHA) in fertilizers. NOTE 2 o,o-EDDHA and o,p-EDDHA are abbreviations used in this European Standard for the sake of simplicity. For complete names see Annex C. NOTE 3 The substances o,o-EDDHA and o,p-EDDHA both exist as different stereoisomers. For o,o-EDDHA a meso form and a d/l pair (the racemic isomers) exist, for o,p-EDDHA two different d/l pairs exist. All four stereoisomers are observed separately in this method. NOTE 4 Currently, an analytically pure standard only exists for o,o-EDDHA. The method for o,p-EDDHA has been developed with an o,p-EDDHA standard containing an uncertain concentration of o,p-EDDHA. 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 3 Principle The technique used is reversed phase HPLC with UV detection at 277 nm. The sample is separated on a silica-based reversed phase column using sodium formate, c = 0,015 mol/l, pH = 3,0, and acetonitrile as mobile phase. For both o,p-EDDHA and o,o-EDDHA, two stereoisomer peaks are observed. The concentration of iron chelated by o,p-EDDHA (o,p-Fe) is determined according to the external standard method. 4 Interferences No interferences have been detected. Iron chelates with EDTA, HEDTA, DTPA and EDDHMA do not interfere. 5 Reagents 5.1 General a) All reagents shall be of recognized analytical grade. SIST EN 15452:2009
EN 15452:2008 (E) 5 b) All water should conform to EN ISO 3696:1995, grade 1. c) When products with a declared purity (P) of less than 99 % are used for the preparation of standard solutions, a correction should be made in order to obtain the required concentration in the solution. 5.2 Sodium hydroxide solution , c(NaOH) = 0,1 mol/l Dissolve 4 g of NaOH in pellet form in water in a 1 000 ml-volumetric flask. Dilute to the mark and homogenize. 5.3 Hydrochloric acid solution, c(HCl) = 4 mol/l Dilute 395 g of concentrated hydrochloric acid (37 %) to 1 000 ml with water. 5.4 Hydrochloric acid solution, c(HCl) = 0,1 mol/l Dilute 25 ml of hydrochloric acid (5.3) to 1 000 ml with water. 5.5 Iron (III) nitrate solution, (Fe) = 4 200 mg/l Dissolve 3,04 g of iron (III) nitrate nonahydrate [Fe(NO3)3.9H2O] in 80 ml of water. Add 1 ml of hydrochloric acid (5.3). Transfer to a 100 ml-volumetric flask. Dilute to the mark with water and homogenize. Check that the Fe concentration of this solution is 4 200 mg/ ± 100 mg/l for example by AAS or iodometric titration. This solution is stable for approximately one week. 5.6 o,p-Fe-EDDHA standard solution, (o,p-Fe) = 100 mg/l Weigh to the nearest 0,1 mg (64,5 ± 1) mg ×100/P, where P is the complexometric purity of the standard in per
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