SIST EN 13368-1:2014

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Düngemittel - Bestimmung von Chelatbildnern in Düngemitteln mit Chromatographie - Teil 1: Bestimmung von EDTA, HEEDTA und DTPA mit IonenchromatographieEngrais - Détermination des agents chélatants dans les engrais par chromatographie - Partie 1: Détermination du EDTA, HEEDTA et DTPA par chromatographie ioniqueFertilizers - Determination of chelating agents in fertilizers by chromatography - Part 1: Determination of EDTA, HEEDTA and DTPA by ion chromatography65.080GnojilaFertilizersICS:Ta slovenski standard je istoveten z:EN 13368-1:2014SIST EN 13368-1:2014en,fr,de01-marec-2014SIST EN 13368-1:2014SLOVENSKI
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SIST EN 13368-1:2014



EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 13368-1
January 2014 ICS 65.080 Supersedes EN 13368-1:2001English Version
Fertilizers - Determination of chelating agents in fertilizers by chromatography - Part 1: Determination of EDTA, HEEDTA and DTPA by ion chromatography
Engrais - Détermination des agents chélatants dans les engrais par chromatographie - Partie 1: Détermination du EDTA, HEEDTA et DTPA par chromatographie ionique
Düngemittel - Bestimmung von Chelatbildnern in Düngemitteln mit Chromatographie - Teil 1: Bestimmung von EDTA, HEEDTA und DTPA mit IonenchromatographieThis European Standard was approved by CEN on 16 November 2013.
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, Former Yugoslav Republic of Macedonia, 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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EN 13368-1:2014 (E) 2 Contents Page Foreword .3 1 Scope .4 2 Normative references .4 3 Terms and definitions .4 4 Principle .4 5 Interferences .4 6 Reagents .5 7 Apparatus .6 8 Sampling and sample preparation .7 9 Procedure .7 9.1 Preparation of the test solution .7 9.2 Preparation of the standard solutions .7 9.3 Chromatographic analysis .7 10 Expression of results .8 11 Precision .8 12 Test report .9 Annex A (informative) Complete names of chelating agents . 10 Annex B (informative) Chromatogram . 11 Bibliography . 12
SIST EN 13368-1:2014



EN 13368-1:2014 (E) 3 Foreword This document (EN 13368-1:2014) 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 2014, and conflicting national standards shall be withdrawn at the latest by July 2014. 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 EN 13368-1:2001. The following modifications have been made: a) the title of the European Standard revised; b) referenced European Standards on vocabulary added to Clause 2; c) Clause 3 Terms and definitions added; d) the sampling method is not part of the standard, informative reference to EN 1482-1 added; e) Annex A: complete names of chelating agents technical revised; f) Bibliography revised; g) editorially revised. 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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. SIST EN 13368-1:2014



EN 13368-1:2014 (E) 4 1 Scope This European Standard specifies a method for the chromatographic determination of the total amount of each of the individual chelating agents EDTA, HEEDTA, and DTPA in fertilizers containing one or more of these substances. The method allows the identification and the determination of the total water soluble fraction of each of these chelating agents. It does not allow to distinguish between the free form and the metal bound form of the chelating agents. NOTE EDTA, HEEDTA and DTPA are abbreviations used in this European Standard for the sake of simplicity. For complete names see Annex A. This method applies to fertilizers containing chelates of one or more of the following micro-nutrients: cobalt, copper, iron, manganese, zinc and with a mass fraction of at least 0,1 %. 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 1482-2, Fertilizers and liming materials - Sampling and sample preparation - Part 2: Sample preparation EN 12944-1:1999, Fertilizers and liming materials and soil improvers - Vocabulary - Part 1: General terms EN 12944-2:1999, Fertilizers and liming materials and soil improvers - Vocabulary - Part 2: Terms relating to fertilizers EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696) 3 Terms and definitions For the purposes of this document, the terms and definitions given in EN 12944-1:1999 and EN 12944-2:1999 apply. 4 Principle The micro-nutrients associated with the chelating agents present in an aqueous extract of the sample are replaced by iron(III). The iron chelates are separated and determined by ion chromatography. The separation is based on anion exchange, by elution with a nitrate acetate solution. The detection is based on UV photometry at 330 nm, after post-column reaction with diluted perchloric acid. 5 Interferences Several substances can interfere, to a degree largely dependent on the type of column used. With the column described in 7.2, the following phenomena have been observed. a) Injection of solutions having high concentrations of salts can cause shifts in the retention times, mostly decreasing the retention when compared to the standard solutions. In these cases, the identity of the peaks can be confirmed by standard addition. SIST EN 13368-1:2014



EN 13368-1:2014 (E) 5 b) Solutions having high concentrations of salts can also create a large signal at the void volume, poorly resolved from the HEEDTA peak. c) High concentrations of nitrate, carbonate, sulfate, and phosphate do not interfere. On the other hand, large amounts of chloride create a negative fronting peak poorly resolved from the DTPA peak, and altering its peak shape. d) Compounds, related to the group of polyamino polycarboxylic acids can interfere. While signals for [o,o] EDDHA, [o,o] EDDHMA, and EDDHSA are not detected, relatively weak signals are observed for NTA and CDTA. Under some conditions NTA may coelute with HEEDTA or EDTA. NOTE EDDHA, EDDHMA, EDDHSA, NTA and CDTA are abbreviations used in this European Standard for the sake of simplicity. For complete names see Annex A. e) No signals have been detected for the following complexing agents: citrate, oxalate, tartrate, phthalate, and 20 naturally occurring amino acids. 6 Reagents 6.1 Reagents of recognized analytical grade and water conforming to EN ISO 3696, degassed by boiling before use. 6.2 Nitric acid, c(HNO3) = 7,2 mol/l. Nitric acid, diluted 1 + 1 with water. 6.3 Sodium hydroxide solution, c(NaOH) = 0,5 mol/l. Dissolve 20 g of NaOH in pellet form in a 1 l volumetric flask with water. Dilute to the mark and homogenize. 6.4 EDTA stock solution, c(EDTA) = 2 mmol/l. Dissolve 372 mg of the disodium dihydrogen salt of ethylene diamine tetraacetic acid dihydrate in 400 ml of water in a 500 ml volumetric flask. After dissolution, dilute to the mark with water and homogenize. Store the solution in a plastic bottle. 6.5 HEEDTA s
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