FprEN 17864

Inorganic fertilizers - Determination of nitrogen content in IBDU (isobutylidenediurea) and CDU (crotonylidenediurea)

This document specifies a method for the determination of nitrogen content in IBDU (isobutylidenediurea) and CDU (crotonylidenediurea) using high-performance liquid chromatography (HPLC).
The method is applicable to all fertilizers which do not contain interfering organic compounds.

Anorganische Düngemittel - Bestimmung des Stickstoffgehalts in IBDU (Isobutylidendiharnstoff) und CDU (Crotonylidendiharnstoff)

Dieses Dokument legt ein Verfahren zur Bestimmung des Stickstoffgehalts in IBDU (Isobutylidendiharnstoff) und CDU (Crotonylidendiharnstoff) durch Hochleistungs-Flüssigkeitschromatographie (en: High Performance Liquid Chromatography [HPLC]) fest.

Engrais inorganiques - Détermination de la teneur en azote dans l'IBDU (isobutylidène diurée) et la CDU (crotonylidène diurée)

Le présent document spécifie une méthode pour la détermination de la teneur en azote dans l’IBDU (isobutylidène diurée) et la CDU (crotonylidène diurée) par chromatographie liquide à haute performance (HPLC).
La méthode est applicable à tous les engrais qui ne contiennent pas de composés organiques interférents.

Anorganska gnojila - Določevanje dušika v IBDU (izobutilidendiurea) in CDU ((krotonilidendiurea)

General Information

• Status: Not Published
• Publication Date: 20-Dec-2023
• ICS: 65.080 - Fertilizers
• Technical Committee: CEN/TC 260 - Fertilizers and liming materials
• Drafting Committee: CEN/TC 260/WG 7 - Chemical analysis
• Current Stage: 5020 - Submission to Vote - Formal Approval
• Start Date: 31-Aug-2023
• Due Date: 04-Dec-2023
• Completion Date: 31-Aug-2023
• Directive: 2019/1009 - Regulation (EU) 2019/1009 of the European Parliament and of the Council of 5 June 2019 laying down rules on the making available on the market of EU fertilising products and amending Regulations (EC) No 1069/2009 and (EC) No 1107/2009 and repealing Regulation (EC) No 2003/2003
• Mandate: M/564 - Fertilising products in support of Regulation (EU) 2019/1009
• Mandate: M/564 AMD 1 - amending Implementing Decision C(2020) 612 as regards certain harmonised standards and standardisation deliverables, deadlines for their adoption and the duration of the validity of the standardisation request
• Ref Project: oSIST prEN 17864:2022 - Inorganic fertilizers - Determination of nitrogen content in IBDU (isobutylidenediurea) and CDU (crotonylidenediurea)

Relations

• Revises: EN 15705:2010 - Fertilizers - Determination of urea condensates using high-performance liquid chromatography (HPLC) - Isobutylidenediurea and crotonylidenediurea (method A) and methylen-urea oligomers (method B)
• Effective Date: 18-Jan-2023

Standards Content (Sample)

SLOVENSKI STANDARD
oSIST prEN 17864:2022
01-julij-2022
Anorganska gnojila - Določevanje dušika v IBDU (izobutilidendiurea) in CDU
((krotonilidendiurea)
Inorganic fertilizers - Determination of nitrogen content in IBDU (isobutylidenediurea) and
CDU (crotonylidenediurea)
Anorganische Düngemittel - Bestimmung des Stickstoffgehalts in IBDU
(Isobutylidendiharnstoff) und CDU (Crotonylidendiharnstoff)
Ta slovenski standard je istoveten z: prEN 17864
ICS:
65.080 Gnojila Fertilizers
oSIST prEN 17864:2022 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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oSIST prEN 17864:2022

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oSIST prEN 17864:2022


DRAFT
EUROPEAN STANDARD
prEN 17864
NORME EUROPÉENNE

EUROPÄISCHE NORM

June 2022
ICS Will supersede
English Version

Inorganic fertilizers - Determination of nitrogen content in
IBDU (isobutylidenediurea) and CDU
(crotonylidenediurea)
 Anorganische Düngemittel - Bestimmung des
Stickstoffgehalts in IBDU (Isobutylidendiharnstoff) und
CDU (Crotonylidendiharnstoff)
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee
CEN/TC 260.

If this draft becomes a European Standard, 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.

This draft European Standard was established by CEN 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, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.

Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are
aware and to provide supporting documentation.

Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without
notice and shall not be referred to as a European Standard.


EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 17864:2022 E
worldwide for CEN national Members.

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oSIST prEN 17864:2022
prEN 17864:2022 (E)
Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 4
5 Reagents . 4
6 Apparatus and equipment . 4
7 Sampling and sample preparation . 5
8 Procedure . 5
9 Calculation and expression of the result . 6
10 Precision . 7
11 Test report . 7
Annex A (informative) Results of the inter-laboratory tests . 8
Annex B (informative) Example chromatogram and calibration curves . 9
Annex C (informative) Example conditions for a suitable HPLC system . 11
Bibliography. 12

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oSIST prEN 17864:2022
prEN 17864:2022 (E)
European foreword
This document (prEN 17864:2022) 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 CEN Enquiry.
This document, together with prEN 15705:2022, will supersede EN 15705:2010.
In comparison with EN 15705:2010, the following technical modifications have been made:
— EN 15705:2010 is split into two parts:
— Method A of EN 15705:2010 is given in this document.
— Method B of EN 15705:2010 is transferred to prEN 15705:2022.
This document has been prepared under a Standardization Request given to CEN by the European
Commission and the European Free Trade Association.
3

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oSIST prEN 17864:2022
prEN 17864:2022 (E)
1 Scope
This document specifies a method for the determination of nitrogen content in IBDU
(isobutylidenediurea) and CDU (crotonylidenediurea) using high-performance liquid chromatography
(HPLC).
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements 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, Fertilizers and liming materials and soil improvers - Vocabulary - Part 1: General terms
EN 12944-2, 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 and EN 12944-2 apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— IEC Electropedia: available at https://www.electropedia.org/
— ISO Online browsing platform: available at https://www.iso.org/obp
4 Principle
The sample is extracted with water and, after appropriate dilution, analyzed using a suitable HPLC
system.
5 Reagents
Use only reagents of recognized analytical grade and distilled or demineralized water, free from carbon
dioxide and all nitrogenous compounds (grade 3 according to EN ISO 3696:1995).
5.1 Acetonitrile, HPLC-grade.
5.2 Isobutylidenediurea (IBDU), in pure form, as standard.
5.3 Crotonylidenediurea (CDU), in pure form, as standard.
5.4 Eluent, acetonitrile + water (10 + 90, V + V).
Mix 100,0 ml of acetonitrile (5.1) with 900,0 ml of water and homogenize well.
6 Apparatus and equipment
Usual laboratory glassware and equipment and, in particular, the following.
4

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oSIST prEN 17864:2022
prEN 17864:2022 (E)
6.1 Analytical balance, capable for weighing to the nearest 0,1 mg.
6.2 Ultrasonic bath.
6.3 Magnetic stirrer.
6.4 Disposable filter, 0,45 μm.
6.5 HPLC-system, with the following components.
6.5.1 UV-detector.
6.5.2 HPLC reversed phase column.
An example of a suitable column and analytical conditions are reported in Annex C.
An acceptable chromatogram, as shown as example in Annex B, can be achieved using a silica column
with C18 reverse phase.
7 Sampling and sample preparation
Sampling is not part of the method specified in this document. A recommended sampling method is given
in EN 1482-1.
Sample preparation s
...