SIST EN 15950:2010

Fertilizers - Determination of N-(1,2-dicarboxyethyl)-D,L-aspartic acid (Iminodisuccinic acid, IDHA) using high-performance liquid chromatography (HPLC)

This European Standard specifies a method for the determination of N-(1,2-dicarboxyethyl)-D,L-aspartic acid (Iminodisuccinic acid (IDHA)) in fertilizers. The method is applicable to all fertilizers containing IDHA as chelating agent for contents > 0,5 % (g/100 g).

Düngemittel - Bestimmung von N-(1,2-Dicarboxyethyl-) D, L Aspartin (Iminodibernsteinsäure (IDHA)) mit Hochleistungs-Flüssigchromatographie (HPLC)

Diese Europäische Norm legt ein Verfahren zur Bestimmung von N-(1,2-Dicarboxyethyl)-D,L-asparaginsäure (Iminodibernsteinsäure, IDHA) in Düngemitteln fest.
Das Verfahren ist auf alle Düngemittel anwendbar, die IDHA als Chelatbildner mit Gehalten von > 0,5 % (g/100 g) enthalten.

Engrais - Dosage de l'acide N-(1,2-dicarboxyéthyl)-D,L aspartique (acide iminodisuccinique, IDHA) par chromatographique liquide haute performance (CLHP)

La présente norme européenne spécifie une méthode de dosage de l’acide N-(1,2-dicarboxyéthyl)-D,L
aspartique (acide iminodisuccinique (IDHA) dans les engrais.
La méthode est applicable à tous les fertilisants contenant de l’IDHA comme agent chélatant dont la teneur
est supérieure à 0,5% (g/100g).

Gnojila - Določevanje N-(1,2-dikarboksietil) D,L asparaginske kisline (iminodijantarna kislina, IDHA) s tekočinsko kromatografijo visoke ločljivosti (HPLC)

Ta evropski standard opredeljuje metodo za določevanje N-(1,2-dikarboksietil) D,L asparaginske kisline (iminodijantarna kislina, IDHA) v gnojilih. Ta metoda se uporablja za vsa gnojila, ki vsebujejo IDHA kot kelatni reagent pri vsebnosti > 0,5 % (g/100 g).

General Information

• Status: Published
• Public Enquiry End Date: 19-Oct-2009
• Publication Date: 18-Nov-2010
• ICS: 65.080 - Fertilizers
• Technical Committee: KAT - Soil quality
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 05-Nov-2010
• Due Date: 10-Jan-2011
• Completion Date: 19-Nov-2010
• Mandate: M/335 - Standardization Mandate assigned to the CEN concerning the modernisation of the methods of anylysis of Fertilizers
• Ref Project: EN 15950:2010 - Fertilizers - Determination of N-(1,2-dicarboxyethyl)-D,L-aspartic acid (Iminodisuccinic acid, IDHA) using high-performance liquid chromatography (HPLC)

Standards Content (Sample)

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.OLQH+3/&Düngemittel - Bestimmung von N-(1,2-Dicarboxyethyl-) D, L Aspartin (Iminodibernsteinsäure (IDHA)) mit Hochleistungs-Flüssigchromatographie (HPLC)Engrais - Dosage de l'acide N-(1,2-dicarboxyéthyl)-D,L aspartique (acide iminodisuccinique, IDHA) par chromatographique liquide haute performance (CLHP)Fertilizers - Determination of N-(1,2-dicarboxyethyl)-D,L-aspartic acid (Iminodisuccinic acid, IDHA) using high-performance liquid chromatography (HPLC)65.080GnojilaFertilizersICS:Ta slovenski standard je istoveten z:EN 15950:2010SIST EN 15950:2010en,fr,de01-december-2010SIST EN 15950:2010SLOVENSKI
STANDARD



SIST EN 15950:2010



EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 15950
October 2010 ICS 65.080 English Version
Fertilizers - Determination of N-(1,2-dicarboxyethyl)-D,L-aspartic acid (Iminodisuccinic acid, IDHA) using high-performance liquid chromatography (HPLC)
Engrais - Dosage de l'acide N-(1,2-dicarboxyéthyl)-D,L aspartique (acide iminodisuccinique, IDHA) par chromatographique liquide haute performance (HPLC)
Düngemittel - Bestimmung von N-(1,2-Dicarboxyethyl)-D,L-asparaginsäure (Iminodibernsteinsäure, IDHA) mit Hochleistungs-Flüssigchromatographie (HPLC) This European Standard was approved by CEN on 4 September 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 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 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 © 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15950:2010: ESIST EN 15950:2010



EN 15950:2010 (E) 2 Contents Page Foreword .31Scope .42Normative references .43Terms and definitions .44Principle .45Interferences .46Reagents .47Apparatus .58Sampling and sample preparation .59Procedure .610Calculation .811Precision for IDHA .812Test report .9Annex A (informative)
Results of the inter-laboratory test . 10Annex B (informative)
Stereo isomers of IDHA, chromatogram and calibration curve . 12B.1Stereo isomers of IDHA . 12B.2Chromatogram . 13B.3Calibration curve. 14Bibliography . 15 SIST EN 15950:2010



EN 15950:2010 (E) 3 Foreword This document (EN 15950:2010) 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 April 2011, and conflicting national standards shall be withdrawn at the latest by April 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 15950:2010



EN 15950:2010 (E) 4 1 Scope This European Standard specifies a method for the determination of N-(1,2-dicarboxyethyl)-D,L-aspartic acid (Iminodisuccinic acid (IDHA)) in fertilizers.
The method is applicable to all fertilizers containing IDHA as chelating agent for contents > 0,5 % (g/100 g). 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 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 3696:1995, Water for analytical laboratory use — Specification and test methods (ISO 3696:1987) 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 IDHA is extracted with water, and measured and detected by reversed phase HPLC using UV detection at 260 nm after total conversion of the chelating agent into its iron-(III)-chelate by adding an excess of a solution of iron-(III)-nitrate (details see Clause 8 and the following). In the HPLC-chromatogram IDHA is represented by two dominant peaks, the first one representing the R,S-isomer (50 %), and the second one representing the R,R- as well as the S,S-isomer (each 25 %). 5 Interferences Other chelating agents such as DTPA, o,o-EDDHA or o,p-EDDHA do not interfere the determination of IDHA. EDTA may interfere with the determination of IDHA with some equipment, especially with certain columns in the HPLC-equipment (see Table A.2). 6 Reagents Use only reagents of recognized analytical grade. 6.1 Water, distilled or demineralized (grade 1 according to EN ISO 3696:1995). 6.2 Tetra-n-butylammonium hydrogen sulfate (C16H37NO4S), for ion pair chromatography. SIST EN 15950:2010



EN 15950:2010 (E) 5 Also tetra-n-butylammonium bromide or -chloride may be used. In that case the pH needs to be adjusted (see 6.9). 6.3 Tetra-n-butylammonium hydroxide, w (C16H37NO) = 40 % in water.
6.4 Iron (III) nitrate nonahydrate, p.a. 6.5 Nitric acid, w(HNO3) = 65 %, p.a. 6.6 Hydrochloric acid, c(HCl) = 1 mol/l and c(HCl) = 0,1 mol/l. 6.7 Sodium hydroxide, c(NaOH) = 1 mol/l and c(NaOH) = 0,1 mol/l. 6.8 Buffer solution, pH = 8,0. Adjust 0,1 mol/l boron as boric/borate buffer at pH = 8,0 with hydrochloric acid or sodium hydroxide. NOTE Commercial buffers may be used. The buffer solution should not contain any phosphate or chelating agents like EDTA or others. 6.9 Eluent solution. In a 1 l volumetric flask dissolve 2,5 g tetra-n-butylammonium hydrogen sulfate (6.2) (= 7,36 mmol), 1,7 ml tetra-n-butylammonium hydroxide (6.3) and 0,04 ml nitric acid (6.5) in water and make up to volume. The pH of this solution is approximately 2,5. In the case that tetra-n-butylammonium bromide or -chloride is used instead of tetra-n-butylammonium hydrogen sulfate, weigh 2,37 g or 2,05 g respectively and adjust pH to approximately 2,5 with additional nitric acid (6.5). 6.10 Derivatisation reagent. In a 100 ml volumetric flask dissolve 4,4 g tetra-n-butylammonium hydrogen sulfate (6.2) (= 12,95 mmol) and 1,5 g iron(III)nitrate nonahydrate (6.4) in water and make up to volume. The pH of this solution is approximately 1,5. In the case that tetra-n-butylammonium bromide or -chloride is used instead of tetra-n-butylammonium hydrogen sulfate, weigh 4,17 g or 3,60 g respectively and adjust pH to approximately 1,5 with additional nitric acid (6.5). 7 Apparatus Laboratory equipment and glassware for preparation of solutions and dilutions. 7.1 Analytical balance, capable of weighing to an accuracy of ± 0,1 mg. 7.2 pH-meter with electro
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