EN 15475:2009
(Main)Fertilizers - Determination of ammoniacal nitrogen
Fertilizers - Determination of ammoniacal nitrogen
This European Standard specifies a method for the determination of the ammoniacal nitrogen content in fertilizers. The method is applicable to all nitrogenous fertilizers including compound fertilizers, in which nitrogen is found exclusively either in the form of ammonium salts or ammonium salts together with nitrates.
This European Standard is not applicable to fertilizers containing urea, cyanamide or other organic nitrogenous compounds.
Düngemittel - Bestimmung von Ammoniumstickstoff
Diese Europäische Norm legt ein Verfahren zur Bestimmung des Ammoniumstickstoffgehalts in Düngemitteln fest. Das Verfahren ist auf alle Stickstoffdünger einschließlich Mehrnährstoffdünger anwendbar, in denen Stickstoff ausschließlich entweder in Form von Ammoniumsalzen oder von Ammoniumsalzen zusammen mit Nitraten enthalten ist.
Diese Europäische Norm gilt nicht für Düngemittel, die Harnstoffe, Cyanamid oder andere organische Stick-stoffverbindungen enthalten.
Engrais - Détermination de l'azote ammoniacal
La présente Norme européenne spécifie une méthode permettant de doser la teneur en azote ammoniacal
dans les engrais. La méthode est applicable à tous les engrais azotés, y compris les engrais composés, dans
lesquels l’azote se trouve exclusivement sous forme de sels d’ammonium ou de sels d’ammonium associés à
des nitrates.
La présente Norme européenne ne s'applique pas aux engrais contenant de l'urée, de la cyanamide ou
d’autres composés organiques azotés.
Gnojila - Določevanje amonijevega dušika
General Information
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Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Düngemittel - Bestimmung von AmmoniumstickstoffEngrais - Détermination de l'azote ammoniacalFertilizers - Determination of ammoniacal nitrogen65.080GnojilaFertilizersICS:Ta slovenski standard je istoveten z:EN 15475:2009SIST EN 15475:2009en,fr,de01-junij-2009SIST EN 15475:2009SLOVENSKI
STANDARDSIST-TS CEN/TS 15475:20061DGRPHãþD
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 15475January 2009ICS 65.080Supersedes CEN/TS 15475:2006
English VersionFertilizers - Determination of ammoniacal nitrogenEngrais - Détermination de l'azote ammoniacalDüngemittel - Bestimmung von AmmoniumstickstoffThis European Standard was approved by CEN on 30 November 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 15475:2009: ESIST EN 15475:2009
Results of the inter-laboratory tests . 14 Bibliography . 15
carbonate free, c = 0,2 mol/l. 5.7 Sulfuric acid (for variant c, see NOTE in 8.2), c = 0,25 mol/l. 5.8 Sodium or potassium hydroxide solution (for variant c, see NOTE in 8.2), carbonate free, c = 0,5 mol/l. 5.9 Sodium hydroxide, 30 %, of approximately ρ(NaOH) = 1,33 g/ml, ammonia free. 5.10 Indicator solutions 5.10.1 Mixed indicator Solution A: Dissolve 1 g of methyl red in 37 ml of sodium hydroxide solution c = 0,1 mol/l and make up to 1 l with water. Solution B: Dissolve 1 g of methylene blue in water and make up to 1 l. Mix one volume of A with two volumes of B. This indicator is violet in acid solution, grey in neutral solution and green in alkaline solution. Use 0,5 ml (10 drops) of this indicator solution.
5.10.2 Methyl red indicator solution Dissolve 0,1 g of methyl red in 50 ml of 95 % ethanol. Make up to 100 ml with water and filter if necessary. This indicator may be used (4 to 5 drops) instead of the preceding one. This indicator is red in acid solution and yellow in alkaline solution. 5.11 Anti-bump granules (i. e. pumice stone, glass pearls), washed in hydrochloric acid and calcined. 5.12 Ammonium sulfate, p. a. 6 Apparatus 6.1 Distillation apparatus
Consisting of a round-bottomed flask of suitable capacity connected to a condenser by means of a splash head. The equipment is made of borosilicate glass. NOTE The different types of equipment recommended for this determination are reproduced, showing all the features of construction in Figures 1, 2, 3 and 4. SIST EN 15475:2009
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
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 (the tap may likewise be replaced by a rubber connection with a clip) Figure 1 — Distillation apparatus 1 SIST EN 15475:2009
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 description Figure 2 — Distillation apparatus 2 SIST EN 15475:2009
Dimensions in millimetres
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 15475:2009
Dimensions in millimetres
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 15475:2009
Sampling is not part of the method specified in this document. A recommended sampling method is given in EN 1482-1. Sample preparation shall be carried out in accordance with EN 1482-2. 8 Procedure 8.1 Preparation of the solution According to Table 1, Table 2 or Table 3, depending on the variant chosen, weigh to the nearest 0,001 g a quantity of 5 g, 7 g, or 10 g of the prepared sample and transfer it into a 500-ml flask. Add 50 ml of water and then 20 ml of hydrochloric acid (5.2). Shake. Leave undisturbed until the evolution of carbon dioxide has ceased. Add 200 ml of water and shake for half an hour with the rotary shaker (6.4). Filter through a filter into a 500-ml graduated flask and make up to the volume with water. 8.2 Analysis of the solution According to the variant chosen, place in the receiving flask a measured quantity of standard sulfuric acid as indicated in Table 1, Table 2 or Table 3. Add the appropriate quantity of the chosen indicator solution (5.10.1 or 5.10.2) and, if necessary, water in order to obtain a volume of at least 50 ml. The end of the extension tube of the condenser shall be below the surface of the solution. Transfer by precision pipette, according to the details given in Table 1, an aliquot portion of the clear solution, into the distillation flask of the apparatus. Add water in order to obtain a total volume of about 350 ml, and several grains of pumice in order to control the boiling. Assemble the distillation apparatus and taking care to avoid any loss of ammonia, add to the contents of the distillation flask 10 ml of concentrated sodium hydroxide solution (5.9) or 20 ml of the sodium hydroxide solution (5.9) in the cases where one has used 20 ml hydrochloric acid (5.2) in order to dissolve the test sample. Gradually warm the flask; avoid boiling vigorously. When boiling commences, distil at a rate of about 100 ml in 10 min to 15 min; the total volume of distillate should be about 250 ml. The condenser shall be regulated so that a continuous flow of condensate is ensured. The distillation should be completed in 30 min to 40 min. When no more ammonia is likely to be evolved, lower the receiving flask so that the tip of the condenser extension is above the surface of
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