CEN/TS 15452:2006
(Main)Fertilizers - Determination of chelating agents - Determination of iron chelated by o,p-EDDHA by reversed phase HPLC
Fertilizers - Determination of chelating agents - Determination of iron chelated by o,p-EDDHA by reversed phase HPLC
This Technical Specification 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 standard for the sake of simplicity. For complete names see Annex A.
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 Presently, 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.
Düngemittel - Bestimmung von Chelatbildnern - Bestimmung von Eisen-chelatisiertem o,p-EDDHA mit Umkehrphasen HPLC
Engrais - Dosage des agents chélatants - Dosage du fer chélaté par o,p-EDDHA par chromatographie liquide à haute performance à polarité de phase inversée
Gnojila - Določevanje sredstev za kelatiziranje - Določevanje železovih kelatov z o,p-EDDHA s tekočinsko kromatografijo visoke ločljivosti (HPLC)
General Information
Relations
Standards Content (Sample)
SLOVENSKI oSIST-TS prCEN/TS
15452:2006
PREDSTANDARD
marec 2006
Gnojila – Določevanje sredstev za kelatiziranje – Določevanje železovih
kelatov z o,p-EDDHA s tekočinsko kromatografijo visoke ločljivosti (HPLC)
Fertilizers - Determination of chelating agents - Determination of iron chelated by
o,p-EDDHA by reversed phase HPLC
ICS 65.080 Referenčna številka
oSIST-TS prCEN/TS 15452:2006(en)
© Standard je založil in izdal Slovenski inštitut za standardizacijo. Razmnoževanje ali kopiranje celote ali delov tega dokumenta ni dovoljeno
TECHNICAL SPECIFICATION
FINAL DRAFT
prCEN/TS 15452
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
January 2006
ICS 65.080
English Version
Fertilizers - Determination of chelating agents - Determination of
iron chelated by o,p-EDDHA by reversed phase HPLC
Engrais - Dosage des agents chélatants - Dosage du fer Düngemittel - Bestimmung von Chelatbildnern -
chélaté par o,p-EDDHA par chromatographie liquide à Bestimmung von Eisen-chelatisiertem o,p-EDDHA mit
haute performance à polarité de phase inversée Umkehrphasen HPLC
This draft Technical Specification is submitted to CEN members for formal vote. It has been drawn up by the Technical Committee CEN/TC
260.
CEN members are the national standards bodies of Austria, Belgium, 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.
: This document is not a Technical Specification. It is distributed for review and comments. It is subject to change without notice
Warning
and shall not be referred to as a Technical Specification.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36 B-1050 Brussels
© 2006 CEN All rights of exploitation in any form and by any means reserved Ref. No. prCEN/TS 15452:2006: E
worldwide for CEN national Members.
prCEN/TS 15452:2006 (E)
Contents Page
Foreword.3
1 Scope .4
2 Normative references .4
3 Principle.4
4 Interferences .4
5 Reagents.4
6 Apparatus .6
7 Sampling and sample preparation.6
8 Procedure .6
9 Expression of results .8
10 Precision.8
Annex A (informative) Complete names of chelating agents .10
Annex B (informative) Typical chromatogram .11
Annex C (informative) Statistical results of the inter-laboratory test .12
Bibliography .13
prCEN/TS 15452:2006 (E)
Foreword
This document (prCEN/TS 15452:2006) has been prepared by Technical Committee CEN/TC 260 “Fertilizers
and liming materials”, the secretariat of which is held by DIN.
This document is currently submitted to the Formal Vote.
This document has been prepared under a mandate given to CEN by the European Commission and the
European Free Trade Association.
prCEN/TS 15452:2006 (E)
1 Scope
This Technical Specification 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 standard for the sake of simplicity. For complete
names see Annex A.
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 Presently, 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.
prEN 1482-1, Fertilizers and liming materials — Sampling and sample preparation — Part 1: Sampling
prEN 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 0,015 M sodium formate, 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.
prCEN/TS 15452:2006 (E)
b) all water should conform to EN ISO 3696.
c) when products with a declared purity 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
ρ(Fe) = 4 200 mg/l
.
Dissolve 3,04 g of iron (III) nitrate nonahydrate [Fe(NO ) 9H O] in 80 ml of water. Add 1 ml of hydrochloric
3 3 2
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 ± 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
ρ(o,p-Fe) = 100 mg/l
c
Weigh to the nearest 0,1 mg (64,5 ± 1)*100/purity (%) mg of o,p-H -EDDHA (m , see 5.1c) in a 100 ml
4 o,p
beaker. Add 5 ml of NaOH (5.2) and carefully dissolve the sample by stirring. Add, after complete dissolution,
35 ml of water and 2,5 ml of iron (III) nitrate solution (5.5). Adjust the pH of the solution to 3,0 with NaOH (5.2)
or HCl (5.4).
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Fertilizers - Determination of chelating agents - Determination of iron chelated by o,p-
EDDHA by reversed phase HPLC
Düngemittel - Bestimmung von Chelatbildnern - Bestimmung von Eisen-chelatisiertem
o,p-EDDHA mit Umkehrphasen HPLC
Engrais - Dosage des agents chélatants - Dosage du fer chélaté par o,p-EDDHA par
chromatographie liquide a haute performance a polarité de phase inversée
Ta slovenski standard je istoveten z: CEN/TS 15452:2006
ICS:
65.080
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
TECHNICAL SPECIFICATION
CEN/TS 15452
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
November 2006
ICS 65.080
English Version
Fertilizers - Determination of chelating agents - Determination of
iron chelated by o,p-EDDHA by reversed phase HPLC
Engrais - Dosage des agents chélatants - Dosage du fer Düngemittel - Bestimmung von Chelatbildnern -
chélaté par o,p-EDDHA par chromatographie liquide à Bestimmung von Eisen-chelatisiertem o,p-EDDHA mit
haute performance à polarité de phase inversée Umkehrphasen HPLC
This Technical Specification (CEN/TS) was approved by CEN on 27 May 2006 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, 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
© 2006 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 15452:2006: E
worldwide for CEN national Members.
Contents Page
Foreword.3
1 Scope .4
2 Normative references .4
3 Principle.4
4 Interferences .4
5 Reagents.4
6 Apparatus .6
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
Foreword
This document (CEN/TS 15452:2006) has been prepared by Technical Committee CEN/TC 260 “Fertilizers
and liming materials”, the secretariat of which is held by DIN.
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 announce this Technical Specification: Austria, Belgium, 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.
1 Scope
This Technical Specification 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 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 Presently, 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.
prEN 1482-2, Fertilizers and liming materials — Sampling and sample preparation — Part 2: Sample
preparation
EN ISO 3696, Water for analytical laboratory use — Specification and test methods (ISO 3696:1987)
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.
b) all water should conform to EN ISO 3696.
c) when products with a declared purity 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
ρ(Fe) = 4 200 mg/l
.
Dissolve 3,04 g of iron (III) nitrate nonahydrate [Fe(NO ) 9H O] in 80 ml of water. Add 1 ml of hydrochloric
3 3 2
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
ρ(o,p-Fe) = 100 mg/l
c
Weigh to the nearest 0,1 mg (64,5 ± 1)*100/purity (%) mg of o,p-H -EDDHA (m , see 5.1c) in a 100 ml
4 o,p
beaker. Add 5 ml of NaOH (5.2) and carefully dissolve the sample by stirring. Add, after complete dissolution,
35 ml of water and 2,5 ml of iron (III) nitrate solution (5.5). Adjust the pH of the solution to 3,0 with NaOH (5.2
...
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