EN 15604:2009

Fertilizers - Determination of different forms of nitrogen in the same sample, containing nitrogen as nitric, ammoniacal, urea and cyanamide nitrogen

This European Standard specifies a method for the determination of any one form of nitrogen in the presence of any other form.
The method is applicable to any fertilizer provided for in Annex I of the Regulation (EC) No 2003/2003 [1] containing nitrogen in various forms.

Düngemittel - Bestimmung verschiedener, nebeneinander anwesender Stickstoff-Formen in derselben Probe mit Stickstoff in Form von Ammonium, Nitrat, Harnstoff und Cyanamid

Diese Europäische Norm legt ein Verfahren zur Bestimmung einer beliebigen Form von Stickstoff in An-wesenheit einer anderen Form von Stickstoff fest.
Das Verfahren ist auf alle Düngemittel anwendbar, die in Anhang I der Verordnung (EG) Nr. 2003/2003 [1] aufgeführt sind, und die Stickstoff in unterschiedlichen Formen enthalten.

Engrais - Détermination des différentes formes d'azote dans un même échantillon contenant l'azote sous forme nitrique, ammoniacale, uréique et cyanamidique

La présente Norme européenne définit une méthode de détermination d’une forme d’azote quelle qu’elle soit en présence d’une autre forme, quelle qu’elle soit.
La méthode s’applique à tout engrais indiqué dans l’Annexe 1 du Règlement (CE) N° 2003/2003 [1] contenant de l’azote sous différentes formes.

Gnojila - Določevanje različnih oblik dušika v istem vzorcu, ki vsebuje dušik v nitratni, amonijevi, sečninski in cianoamidni obliki

General Information

• Status: Published
• Publication Date: 20-Jan-2009
• ICS: 65.080 - Fertilizers
• Technical Committee: CEN/TC 260 - Fertilizers and liming materials
• Drafting Committee: CEN/TC 260/WG 7 - Chemical analysis
• Current Stage: 9093 - Decision to confirm - Review Enquiry
• Start Date: 05-Feb-2025
• Completion Date: 14-Apr-2025
• Mandate: M/335 - Standardization Mandate assigned to the CEN concerning the modernisation of the methods of anylysis of Fertilizers
• Ref Project: SIST EN 15604:2009 - Fertilizers - Determination of different forms of nitrogen in the same sample, containing nitrogen as nitric, ammoniacal, urea and cyanamide nitrogen

Relations

• Replaces: CEN/TS 15604:2007 - Fertilizers - Determination of different forms of nitrogen in the same sample, containing nitrogen as nitric, ammoniacal, urea and cyanamide nitrogen
• Effective Date: 08-Jun-2022

Overview

EN 15604:2009 (CEN) - Fertilizers - Determination of different forms of nitrogen in the same sample, containing nitrogen as nitric, ammoniacal, urea and cyanamide nitrogen.

This European Standard specifies analytical procedures to determine any one form of nitrogen when multiple nitrogen forms coexist in a fertilizer sample. It applies to fertilizers listed in Annex I of Regulation (EC) No 2003/2003 that contain nitrogen in various chemical forms. The method is intended for reliable measurement of total soluble/insoluble nitrogen and of individual soluble fractions (nitrate, ammoniacal, urea, cyanamide) taken from the same prepared aliquot.

Key topics and technical requirements

• Scope and applicability: Applicable to fertilizers with mixed nitrogen forms (nitric/nitrate, ammoniacal, urea, cyanamide) as defined by Regulation (EC) No 2003/2003.
• Analytical principle: Uses a combination of Kjeldahl digestion and selective reduction/pretreatment to convert and quantify specific nitrogen forms from the same sample solution.
  • Direct Kjeldahl digestion for samples without nitrates.
  • Kjeldahl digestion after reduction (metallic iron and stannous chloride / Ulsch reduction) when nitrates are present.
• Fraction determination:
  • Total soluble and insoluble nitrogen (with note on insoluble N > 0.5% indicating unexpected nitrogen forms).
  • Ammoniacal nitrogen: determined by distillation/absorption and titration in accordance with EN 15475.
  • Nitrate nitrogen: typically determined by difference between total N measures or specific elimination steps.
  • Urea nitrogen: by enzymatic conversion with urease to ammonia, by xanthydrol gravimetry, or by difference (method selection depends on matrix).
  • Cyanamide nitrogen: precipitated as a silver compound and determined by Kjeldahl on the precipitate.
• Reagents and apparatus: Specifies reagent quality (analytical grade, grade 3 water per EN ISO 3696), reducing agents, catalysts, indicators and glassware; includes guidance on distillation and digestion apparatus.
• Sampling and sample prep: Sampling not included in method; sample preparation referenced to EN 1482-2.

Applications and users

• Who uses EN 15604:2009:
  • Fertilizer manufacturers and formulators for product characterization and quality control.
  • Independent testing laboratories performing statutory or customer-required analyses.
  • Regulatory bodies verifying compliance with EU fertilizer legislation (Regulation (EC) No 2003/2003).
  • R&D teams developing blended fertilizers containing multiple nitrogen sources.
• Practical value:
  • Enables accurate split of nitrogen species in complex fertilizer matrices.
  • Supports compliance testing, labeling accuracy, and agronomic dosing recommendations.

Related standards

• EN 15475 - Determination of ammoniacal nitrogen
• EN 15562 - Determination of cyanamide nitrogen
• EN 1482-2 - Sample preparation for fertilizers
• EN ISO 3696 - Water for analytical laboratory use

Keywords: EN 15604:2009, fertilizer nitrogen determination, ammoniacal nitrogen, nitrate nitrogen, urea nitrogen, cyanamide nitrogen, Kjeldahl method, CEN standard.

Standards Content (Sample)

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Düngemittel - Bestimmung verschiedener, nebeneinander anwesender Stickstoff-Formen in derselben Probe mit Stickstoff in Form von Ammonium, Nitrat, Harnstoff und CyanamidEngrais - Détermination des différentes formes d'azote dans un même échantillon contenant l'azote sous forme nitrique, ammoniacale, uréique et cyanamidiqueFertilizers - Determination of different forms of nitrogen in the same sample, containing nitrogen as nitric, ammoniacal, urea and cyanamide nitrogen65.080GnojilaFertilizersICS:Ta slovenski standard je istoveten z:EN 15604:2009SIST EN 15604:2009en,fr,de01-junij-2009SIST EN 15604:2009SLOVENSKI
STANDARDSIST-TS CEN/TS 15604:20081DGRPHãþD

EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 15604January 2009ICS 65.080Supersedes CEN/TS 15604:2007
English VersionFertilizers - Determination of different forms of nitrogen in thesame sample, containing nitrogen as nitric, ammoniacal, ureaand cyanamide nitrogenEngrais - Détermination des différentes formes d'azotedans un même échantillon contenant l'azote sous formenitrique, ammoniacale, uréique et cyanamidiqueDüngemittel - Bestimmung verschiedener, nebeneinanderanwesender Stickstoff-Formen in derselben Probe mitStickstoff in Form von Ammonium, Nitrat, Harnstoff undCyanamidThis European Standard was approved by CEN on 6 December 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© 2009 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15604:2009: ESIST EN 15604:2009

Key 1 round-bottomed, long-necked flask of 1 000 ml capacity 2 distillation tube with a splash head, connected to the condenser by means of a spherical joint (No 18) (the spherical joint for the connection to the condenser may be replaced by an appropriate rubber connection) 3 funnel with a polytetrafluoroethylene (PTFE) tap (6) for the addition of sodium hydroxide (the tap may likewise be replaced by a rubber connection with a clip) 4 six-bulb condenser with spherical joint (No 18) at the entrance, and joined at the issue to a glass extension tube by means of a small rubber connection (when the connection to the distillation tube is effected by means of a rubber tube, the spherical joint may be replaced by a suitable rubber bung) 5 500 ml flask in which the distillate is collected 6 PTFE tap a hole Figure 1 — Distillation apparatus 1 SIST EN 15604:2009

Key 1 round-bottomed, short-necked flask of 1 000 ml capacity with a spherical joint (No 35) 2 distillation tube with a splash head, equipped with a spherical joint (No 35) at the entrance and a spherical joint (No 18) at the issue, connected at the side to a funnel with a polytetrafluoroethylene (PTFE) tap (5) for the addition of sodium hydroxide 3 six-bulb condenser with a spherical joint (No 18) at the entrance and joined at the issue to a glass extension tube by means of a small rubber connection 4 500 ml flask in which the distillate is collected 5 PTFE tap a enlarged cross-section Figure 2 — Distillation apparatus 2 SIST EN 15604:2009

Key 1 round-bottomed, long-necked flask of 750 ml or 1 000 ml capacity with a bell mouth 2 distillation tube with a splash head and a spherical joint (No 18) at the issue 3 elbow tube with a spherical joint (No 18) at the entrance, and a drip cone (the connection to the distillation tube may be effected by means of a rubber tube instead of a spherical joint) 4 six-bulb condenser joined at the issue to a glass extension tube by means of a small rubber connection 5 500 ml flask in which the distillate is collected Figure 3 — Distillation apparatus 3 SIST EN 15604:2009

Key 1 round-bottomed, long-necked flask of 1 000 ml capacity with a bell mouth 2 distillation tube with a splash head and a spherical joint (No 18), at the issue, connected at the side to a funnel with a polytetrafluoroethylene (PTFE) tap (5) for the addition of sodium hydroxide (a suitable rubber bung may be used instead of the spherical joint; the tap may be replaced by a rubber connection with an appropriate clip) 3 six-bulb condenser with a spherical joint (No 18) at the entrance, joined at the issue, by a rubber connection, to a glass extension tube (when the connection to the distillation tube is effected by means of a rubber tube, the spherical joint may be replaced by a suitable rubber bung) 4 500 ml flask for the collection of the distillate 5 PTFE tap Figure 4 — Distillation apparatus 4 SIST EN 15604:2009

6.2 Apparatus for the determination of ammoniacal nitrogen According to analytical technique (8.2.5.3). The apparatus is made up of a specially shaped receptacle with a ground glass neck, with a side neck, a connecting tube with a splash head and a perpendicular tube for the introduction of air. The tubes can be connected to the receptacle by means of a simple perforated rubber bung. It is important to give a suitable shape to the end of the tubes introducing air, since the bubbles of gas should be evenly distributed throughout the solutions contained in the receptacle and the absorber. The best arrangement consists of small mushroom-shaped pieces with an external diameter of 20 mm and six openings of 1 mm around the periphery. 6.3 Apparatus for the determination of urea nitrogen According to the urease technique (8.2.6.1). It consists of a 300 ml Erlenmeyer flask, with a separating funnel and a small absorber. 6.4 Rotary shaker, 35 to 40 revolutions per min. 6.5 pH meter 6.6 Oven, capable of being maintained at a temperature of 130 °C. 6.7 Glassware: a) pipettes of 2 ml, 5 ml, 10 ml, 20 ml, 25 ml, 50 ml and 100 ml capacity; b) long-necked Kjeldahl flasks of 300 ml and 500 ml capacity; c) graduated flasks of 100 ml, 250 ml, 500 ml and 1 000 ml capacity; d) crucibles of sintered glass, pore diameter, 5 µm to 15 µm; e) mortars. 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 [2]. Sample preparation shall be carried out in accordance with EN 1482-2. SIST EN 15604:2009
...