Inorganic fertilizers - Determination of total nitrogen in calcium cyanamide containing nitrates

This document specifies a method for the determination of total nitrogen in calcium cyanamide. The method is applicable to calcium cyanamide containing nitrates.

Anorganische Düngemittel - Bestimmung des Gesamtstickstoffs in nitrathaltigem Kalkstickstoff

Dieses Dokument legt ein Verfahren zur Bestimmung von Gesamtstickstoff in Kalkstickstoff (Calcium-cyanamid) fest. Das Verfahren ist auf Nitrate enthaltenden Kalkstickstoff anwendbar.

Engrais - Dosage de l'azote total dans la cyanamide calcique nitratée

Le présent document spécifie une méthode de détermination de l’azote total dans la cyanamide calcique nitratée. La méthode est applicable à la cyanamide calcique contenant des nitrates.

Gnojila - Določevanje celotnega dušika v kalcijevem cianoamidu, ki vsebuje nitrate

General Information

Status
Not Published
Publication Date
19-Jul-2023
Current Stage
5060 - Closure of Vote - Formal Approval
Start Date
25-May-2023
Due Date
04-May-2023
Completion Date
25-May-2023

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SLOVENSKI STANDARD
oSIST prEN 15561:2021
01-december-2021

Gnojila - Določevanje celotnega dušika v kalcijevem cianoamidu, ki vsebuje nitrate

Fertilizers - Determination of total nitrogen in calcium cyanamide containing nitrates

Düngemittel - Bestimmung des Gesamtstickstoffs in nitrathaltigem Kalkstickstoff
Engrais - Détermination de l'azote total dans la cyanamide calcique nitratée
Ta slovenski standard je istoveten z: prEN 15561
ICS:
65.080 Gnojila Fertilizers
oSIST prEN 15561:2021 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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oSIST prEN 15561:2021
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oSIST prEN 15561:2021
DRAFT
EUROPEAN STANDARD
prEN 15561
NORME EUROPÉENNE
EUROPÄISCHE NORM
November 2021
ICS 65.080 Will supersede EN 15561:2009
English Version
Fertilizers - Determination of total nitrogen in calcium
cyanamide containing nitrates

Engrais - Détermination de l'azote total dans la Düngemittel - Bestimmung des Gesamtstickstoffs in

cyanamide calcique nitratée nitrathaltigem Kalkstickstoff

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

© 2021 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 15561:2021 E

worldwide for CEN national Members.
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oSIST prEN 15561:2021
prEN 15561:2021 (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 ................................................................................................................. 5

Figure 1 — Distillation apparatus 1 ............................................................................................................. 6

Figure 2 — Distillation apparatus 2 ............................................................................................................. 7

Figure 3 — Distillation apparatus 3 ............................................................................................................. 8

Figure 4 — Distillation apparatus 4 ............................................................................................................. 9

7 Sampling and sample preparation ............................................................................................... 10

8 Procedure .............................................................................................................................................. 10

8.1 Preparation of the solution ............................................................................................................. 10

8.2 Analysis of the solution ..................................................................................................................... 10

Table 1 — Weighing, dilution and calculation variants a, b and c ................................................... 11

8.3 Blank ........................................................................................................................................................ 11

8.4 Control test ............................................................................................................................................ 11

9 Calculation and expression of the result .................................................................................... 11

10 Test report ............................................................................................................................................. 12

Bibliography ....................................................................................................................................................... 13

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oSIST prEN 15561:2021
prEN 15561:2021 (E)
European foreword

This document (prEN 15561:2021) 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 will supersede EN 15561:2009.

In comparison with the previous edition, the following technical modifications have been made:

— technical change to the preparation of the solution, i.e. deletion of the last paragraph of 8.1;

— deletion of former tables and addition of a technically revised Table (8.2).
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oSIST prEN 15561:2021
prEN 15561:2021 (E)
1 Scope

This document specifies a method for the determination of total nitrogen in calcium cyanamide.

The method is applicable to calcium cyanamide containing nitrates.
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
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

Reduction of nitrate nitrogen to ammonia with metallic iron and stannous chloride solution. Digestion in

sulfuric acid. Distillation of the ammonia from an alkaline solution, absorption in an excess of standard

sulfuric acid solution and back-titration with standard sodium or potassium hydroxide solution.

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 Sulfuric acid, mass concentration ρ = 1,84 g/ml.
5.2 Powdered iron, reduced in hydrogen.
5.3 Potassium sulfate, analytical grade, finely pulverized.
5.4 Sulfuric acid (for variant a), substance concentration c = 0,05 mol/l.

5.5 Sodium or potassium hydroxide standard solution (for variant a), carbonate free, c = 0,1 mol/l.

5.6 Sulfuric acid (for variant b), c = 0,1 mol/l.

5.7 Sodium or potassium hydroxide standard solution (for variant b), carbonate free, c = 0,2 mol/l.

5.8 Sulfuric acid (for variant c), c = 0,25 mol/l.
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oSIST prEN 15561:2021
prEN 15561:2021 (E)

5.9 Sodium or potassium hydroxide standard solution (for variant c), carbonate free, c = 0,5 mol/l.

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 (5.6) 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 solution A with two volumes of solution 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 that specified in 5.10.1.
5.11 Stannous chloride solution

Dissolve 120 g of SnCl •2HO in 400 ml of concentrated hydrochloric acid (density at 20 °C

2 2

ρ = 1,18 g/ml) and make up to 1 l with water. The solution shall be completely clear and prepared

immediately before use.

It is essential to check the reducing power of the stannous chloride: dissolve 0,5 g of SnCl •2H O in 2 ml

2 2

of concentrated hydrochloric acid (ρ = 1,18 g/ml) and make up to 50 ml with water. Then add 5 g of

Rochelle salt (potassium sodium tartrate), then a sufficient quantity of sodium bicarbonate for the

solution to be alkaline to litmus paper.
Titrate with an iodine s
...

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