BS en 15562-2023 - TC Tracked Changes. Inorganic Fertilizers. Determination of Cyanamide Nitrogen.

BS ISO
BS EN EN 15562:2023
13850:2015 — Tracked Changes
compares
compares BS 15562:2023
BS EN 13850:2015
withwith
BS EN
BS 15562:2009
13850:2008
BSI Standards
BSI StandardsPublication
Publication
Inorganic fertilizers –—Emergency

Safety of machinery Determination
stop of
cyanamide nitrogen for design
function – Principles
TRACKED CHANGES
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this document, should be considered the version of record for
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This is a tracked changes copy and uses the following colour coding:
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About Tracked Changes

This document is a PDF containing a Tracked Changes version of
BS EN 15562, which compares BS EN 15562:2023 with
BS EN 15562:2009.
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© The British Standards Institution 2023

Published by BSI Standards Limited 2023
ISBN 978 0 539 28464 5
Amendments/corrigenda issued since publication

Date Text affected
BS EN 15562:2023 — Tracked Changes
National foreword
This British Standard is the UK implementation of
EN 15562:2009. It supersedes DD CEN/TS 15562:2007 which
is withdrawn.
The UK participation in its preparation was entrusted to

Technical Committee CII/37, Fertilisers and related chemicals.
A list of organizations represented on this committee can be

obtained on request to its secretary.
This publication does not purport to include all the necessary

provisions of a contract. Users are responsible for its correct
application.
Compliance with a British Standard cannot confer

immunity from legal obligations.
This British Standard was published under the authority of the

Standards Policy and Strategy Committee on 30 June 2009
Date Comments
National foreword
This British Standard is the UK implementation of EN 15562:2023.
It supersedes BS EN 15562:2009, which is withdrawn.
The UK participation in its preparation was entrusted to Technical
Committee CII/37, Fertilisers and related chemicals.
A list of organizations represented on this committee can be
obtained on request to its committee manager.
Contractual and legal considerations
This publication has been prepared in good faith, however no
representation, warranty, assurance or undertaking (express or
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This publication is not intended to constitute a contract. Users are
responsible for its correct application.
ISBN 978 0 580 62390 5978 0 539 18858 5
ICS 65.080
Compliance with a British Standard cannot confer immunity
from legal obligations.
Standards Policy and Strategy Committee on 31 August 2023.
Date Text affected

EUROPEAN STANDARD BS EN 15562
EUROPEAN STANDARD EN ISO 13850
NORME EUROPÉENNE
NORME EUROPÉENNE
EUROPÄISCHE NORM August 2023
EUROPÄISCHE NORM June 2008November 2015
ICS 65.080 Supersedes BS EN 15562: 2009
ICS 13.110 Supersedes EN ISO 13850:20068
English Version
English Version
Fertilizers — Determination of cyanamide nitrogenInorganic
Safety of machinery
fertilizers - Emergency
- Determination ofstop functionnitrogen
cyanamide - Principles
for design (ISO 13850:200615)
Engrais — Détermination de l'azote cyanamidéEn- Düngemittel — Bestimmung von Cyanamidstickstof-
grais inorganiques - Dosage de l'azote cyanamidé fAnorganische Düngemittel - Bestimmung des Cyana-
Sécurité des machines - ArrêtFonction d'arrêt d'urgence - Sicherheit von midstickstoffs
Maschinen - Not-Halt -
Principes de conception (ISO 13850:200615) Gestaltungsleitsätze (ISO 13850:200615)
This European Standard was approved by CEN on 6 December 200826 June 2023.
This European Standard was approved by CEN on 25 May 20085 September 2015.
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. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
concerning
member. such national standards may be obtained on application to the CEN-CENELEC 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
This European
translation Standard
under exists in three
the responsibility of aofficial versionsinto
CEN member (English,
its ownFrench, German).
language A version
and notified in CEN-CENELEC
to the any other language made by
Management
translation under the responsibility of a CEN member
Centre has the same status as the official versions. 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,
CEN members
Estonia, Finland, the national
areFrance, standards
Germany, bodies
Greece, of Austria,
Hungary, Iceland,Belgium,
Ireland,Bulgaria, Croatia,
Italy, Latvia, Cyprus,Luxembourg,
Lithuania, Czech Republic, Denmark,
Malta, Estonia,
Netherlands,
Finland,
Norway, Former
Poland, Yugoslav
Portugal,Republic
RepublicofofMacedonia, France,Romania,
North Macedonia, Germany,Serbia,
Greece,Slovakia,
Hungary,Slovenia,
Iceland, Spain,
Ireland, Italy, Latvia,
Sweden, Lithuania,
Switzerland,
Luxembourg, Malta, Kingdom.
Türkiye and United Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.
EUROPEANCOMMITTEE
EUROPEAN COMMITTEE FORFOR STANDARDIZATION
STANDARDIZATION
COMITÉ
COM EUROPÉEN
I T É EUROPÉ DENOR
E N DE NORMALISATION
M ALISATI ON
EUROPÄISCHES
E UR KOMITEE
O PÄI SC HE S KO FÜR N
M I T E E FÜR NORMUNG
O R M UNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
CEN-CENELEC Management Centre: rue de Stassart, 36Avenue Marnix 17, B-10500 Brussels
© 20092023CEN/ All rights of exploitation in any form and by any means reserved Ref. No. BS EN 15562: 20092023 E
CENELEC worldwide for CEN national Members.All rights of exploitation in any
© 200815 CEN Allform
rights
andof by
exploitation
any meansin any form
reserved and by any
worldwide formeans reserved
CEN national Ref. No. EN ISO 13850:2008:2015 E
worldwide
Membersfor CEN national Members.
ForewordEuropean foreword
This document (EN 15562:2009EN 15562:2023) has been prepared by Technical
Committee CEN/TC 260 “Fertilizers and liming materials”, the secretariat of which is held
by DIN.
This European Standard shall be given the status of a national standard, either by
publication of an identical text or by endorsement, at the latest by July 2009February
2024, and conflicting national standards shall be withdrawn at the latest by July
2009February 2024.
Attention is drawn to the possibility that some of the elements of this document may be
the subject of patent rights. CEN [and/or CENELEC] shall not be held responsible for
identifying any or all such patent rights.
This document supersedes CEN/TS 15562:2007EN 15562:2009.
In comparison with the previous edition EN 15562:2009, the following technical

modifications have been made:
— t echnical changes have been made to the description of the procedure (Clause 8) and
to Table 1 (8.2);
— deletion of distillation apparatus drawings.
This document has been prepared under a mandate givenstandardization request

addressed to CEN by the European Commission and. The Standing Committee of the
European Free Trade AssociationEFTA States subsequently approves these requests for
its Member States.
Any feedback and questions on this document should be directed to the users’ national
standards body. A complete listing of these bodies can be found on the CEN website.
According to the CEN/-CENELEC Internal Regulations, the national standards

organizationsorganisations of the following countries are bound to implement this
European Standard: 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, Türkiye and
the United Kingdom.
Contents Page
1 Scope��1
2 Normative references��1
3 Terms and definitions��1
4 Principle��1
5 Reagents��2
5.1 Glacial acetic acid�� 2
5.6 Catalyst�� 2
5.9 Indicator solutions�� 2
5.9.1 Mixed indicator�� 2
5.9.2 Methyl red indicator�� 3
6 Apparatusand equipment ��3
7 Sampling and sample preparation��8
8 Procedure��8
8.1 Preparation of the solution for analysis�� 8
8.2 Analysis of the solution�� 8
8.3 Blank test��10
8.4 Control test��10
9 Expression of the result�� 10
10 Test report�� 11
Bibliography�� 12
© BSI 2023 – All rights reserved vii

This page is left intentionally blank
INTERNATIONAL STANDARD
1 Scope
This European Standarddocument specifies a method for the determination of cyanamide

nitrogen in fertilizers. The method is applicable to calcium cyanamide and mixtures of
calcium cyanamide/nitrate mixtures with calcium nitrate.
2 Normative references
The following referenced documents are indispensable forreferred to in the applicationtext

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 12944‑1:1999EN 12944‑1, Fertilizers and liming materials and soil improvers —

Vocabulary — Part 1: General terms
EN 12944‑2:1999, Fertilizers and liming materials and soil improvers — Vocabulary —

Part 2: Terms relating to fertilizers
EN ISO 3696:1995EN 12944‑2, Water for analytical laboratory use Fertilizers and liming
materials — Specification and test methods (ISO 3696:1987)Vocabulary — Part 2: Terms
relating to fertilizers
3 Terms and definitions
For the purposes of this document, the terms and definitions given in
EN 12944‑1:1999EN 12944‑1 and EN 12944‑2:1999EN 12944‑2 apply.
ISO and IEC maintain terminology databases for use in standardization at the following
addresses:
• I EC Electropedia: available at https://www.electropedia.org/
• I SO Online browsing platform: available at https://www.iso.org/obp
4 Principle
Precipitation of cyanamide nitrogen as a silver complex. Digestion in sulfuric acid with

the aid of a catalyst. Distillation of the ammonia from an alkaline solution, absorption in
an excess of standard sulfuric acid volumetric solution and back-titration with standard
sodium or potassium hydroxide volumetric solution.
© BSI 2023 – All rights reserved 1

5 Reagents
5.1 General
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).
Use only reagents of recognized analytical grade and water with an electrical
conductivity < 0,5 mS/m (at 25 °C).
5.25.1 Glacial acetic acid
5.35.2 Ammonia solution, containing 10 % of ammonia gas by mass (, ρ 20 = 0,96 g/ml).
5.45.3 Ammoniacal silver solution, according to Tollens.
Mix 500 ml of 10 % silver nitrate (AgNO 3) solution in water with 500 ml of 10 % ammonia
solution (5.35.2).
Do not expose unnecessarily to light, heat or air. The solution normally keeps for years. As
long as the solution remains clear, the reagent is of good quality.
5.55.4 Concentrated sulfuricSulfuric acid, mass concentration ρ 20 = 1,84 g/ml.
5.65.5 Potassium sulfatesulphate, p.a.analytical grade
5.75.6 Catalyst
Use 0,3 g to 0,4 g of copper (II) oxide or 0,95 g to 1,25 g of copper (II) sulfatesulphate
pentahydrate for each determination.
5.8 Sodium hydroxide solution, approximately 30 % NaOH (ρ 20 = 1,33 g/ml), ammonia

free.
5.95.7 Sulfuric acid, substance concentration c = 0,05 mol/l.
5.105.8 Sodium or potassium hydroxide solution,, substance concentration

c = 0,1 mol/l., carbonate free
5.115.9 Indicator solutions
5.11.15.9.1 Mixed indicator
Solution A: Dissolve 10,1 g of methyl red in 373,7 ml of sodium hydroxide solutionor

potassium hydroxide, c = 0,1 mol/l (5.8) and make up to 1 l100 ml with water.
Solution B: Dissolve 10,1 g of methylene blue in water and make up to 1 l100 ml.
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.
2 © BSI 2023 – All rights reserved

5.11.25.9.2 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
5.11.15.9.1.
5.10 Sodium hydroxide, 30 % m/v, mass concentration, ρ 20 = 1,33 g/ml, ammonia free
5.125.11 Anti-bump granules of pumice stone, (i.e. pumice stone, glass pearls),
washed in hydrochloric acid and calcined.
5.135.12 Potassium thiocyanate, (mass fraction w N = 14,4 %), for the control test.
analytical grade
6 Apparatus and equipment
Usual laboratory glassware and equipment and, in particular, the following.
6.1 Distillation apparatus
Consisting Distillation apparatus, according to Kjeldahl, 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.
Automatic distillation apparatus may be used also, provided that the results are statistically
equivalent.
Dimensions in millimetres

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

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

5 PTFE-tap
a
enlarged description

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

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
6.2 Graduated flask, capacity 500 ml.
6.3 Long-necked Kjeldahl flask, long necked and of suitable capacity (300 ml to
500 ml).
6.4 Pipette, capacity 25 ml and 50 ml.
6.5 Rotary shaker, 35 turns to 40 turns per minute.
6.6 Graduated burette, 50 ml. (div. 1/10)
7 Sampling and sample preparation
Sampling is not part of the method specified in this European Standarddocument. A

recommended sampling method is given in EN 1482‑1.
Sample preparation shall be carried out in accordance with EN 1482‑2.
8 Procedure
SAFETY PRECAUTIONS – When using any ammoniacal silver solution safety goggles
shall be worn. As soon as a thin membrane forms on the surface of the liquid, an
explosion can be produced by agitation and the greatest caution is essential.
WARNING — When using any ammoniacal silver solution safety goggles shall be worn. As soon as a thin
membrane forms on the surface of the liquid, an explosion can be produced by agitation and the greatest
caution is essential.
8.1 Preparation of the solution for analysis
WeighAccording to Table 1, weigh, to the nearest 0,001 g, about 2,5 g of the

preparedprescribed quantity of sample and place it in a smallsuitable glass mortar. Grind
the sample three times with water, pouring off the water after each grinding into a 500 ml
graduated flask (6.2). Transfer quantitatively the sample into the 500 ml graduated flask
(6.2), washing the mortar, pestle and funnel with water. Make up with water to
approximately 400 ml. Add 15 ml of acetic acid (5.25.1). Shake on the rotary shaker (6.5)
for approximately 2 h.
Make up to 500 ml with water, mix and filter.
The analysis shall be carried out as quickly as possible.
8.2 Analysis of the solution
Transfer 50 mlAccording to Table 1, transfer with a pipette (6.4) the prescribed volume of
the filtrate into a 250 ml beaker.
Add ammonia solution (5.35.2) until slightly alkaline and add 30 ml of warm ammoniacal
silver nitrate (5.45.3) in order to precipitate the yellow silver complex of the cyanamide.

Leave overnight, filter and wash the precipitate with cold water until it is completely free
of ammonia.
Place the filter and the precipitate, still moist, in a Kjeldahl flask (6.3), add 10 g to 15 g of
potassium sulfatesulphate (5.65.5), the appropriate amount of the catalyst (5.75.6), in the
prescribed proportion, then 50 ml of water and 25 ml of concentrated sulfuric acid
(5.55.4).
Warm the flask slowly, while shaking it gently until the contents come to the boil. Increase
the heat, boil until the contents of the flask become colourless or pale green.
Continue boiling for approximately 1 h, then leave to cool.
Slowly add 100 ml to 150 ml of water with a gentle swirling. Wait the solution to cool.
Place Using a graduated burette (6.6), place in the receiving flask 50 ml of standard
sulfuric acid 0,05 mol/l (5.7). Add the appropriate quantity of the chosen indicator
solution (5.11.15.9.1 or 5.11.25.9.2) and, if necessary, water in order to obtainget 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 toQuantitatively transfer the details given in

Table 1, an aliquot portion of the cleardigested solution, into the distillation flask of the
apparatus (6.1). Add water in order to obtainget a total volume of about 350 ml and several
grains of pumice in order (5.11) to control the boiling.
Assemble the distillation apparatus (6.1) and, taking care to avoid any loss of ammonia,
add to the contents of the distillation flask 200 ml of 30 % m/v sodium hydroxide (5.10).
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
(5.8) (add sufficient NaOH solution (5.8) to ensure the presence of a considerable excess).
Gradually warm the flask, to avoidand when boiling vigorously. When boiling
commencesbegins, distil at the 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 the liquid.
Test the subsequent distillate by means of an appropriate reagent to ensure that all the
ammonia is completely distilled. Wash the condenser extension with a little water and
titrate the surplus acid with the standard solution of sodium or potassium hydroxide (see
NOTE).
NOTE Standard solutions of different strengths may be used for the back-titration provided that the
volumes used for the titration do not, as far as possible, exceed 45 ml.
Titrate the excess of sulphuric acid (5.7) with the sodium or potassium hydroxide (5.8)
using a graduated burette (6.6), until the solution turns from purple to grey using the
mixed indicator (5.9.1).

Table 1 Weighing, dilution and calculationdilution
Declaration Amount Solution of

wN to be Dilution sample to be Expression of the result a
weighed distilled
% g ml ml w N = (50 ±V ) F
0 to 5 10 500 50 (50 – V ) × 0,14
5 to 10 10 500 25 (50 – V ) × 0,28
10 to 15 7 500 25 (50 – V ) × 0,40
15 to 20 5 500 25 (50 – V ) × 0,56
20 to 40 7 500 10 (50 – V ) × 1,00
Approximate maximum quantity of nitrogen to be distilled: 50 mg.
Back-titration with NaOH or KOH 0,1 mol/l.
a
For the purposes of the equation for expression of the result:
— 0 is the volume of the standard solution of sulfuric acid to be placed in the receiving flask, in
5
millilitres;
— V is the volume of the sodium or potassium hydroxide used for the back titration;
— F is the factor comprising the amount weighed, the dilution, the aliquot part of solution of the
sample to be distilled and the volumetric equivalent.
Declaration N% Amount to be Dilution Solution of sample to be Dilution factor

weighed digested and distilled
g ml ml
0 to 5 10 500 50 10
5 to 10 10 500 25 20
10 to 20 5 500 25 20
8.3 Blank test
Carry out a blank test (omitting the sample) under the same conditions and refer to this
in the calculation of the final result.
8.4 Control test
Before carrying out the analysis, check that the apparatus is working properly and that
the correct technique is applied using an aliquot part of a standard solutionweighing, to
the nearest 0,001 g, 5 g of potassium thiocyanate (5.135.12) corresponding to 0,05 g of
nitrogenand proceeding as in 8.1 and 8.2.
9 Calculation and expressionExpression of the result
Calculate the content of cyanamide nitrogen as a percentage mass fraction of the fertilizer
as received for analysis according to Table 1Formula (1).:
(1)
where

VB is the volume of sodium or potassium hydroxide 0,1 mol/l used for the blank, in ml;
VS is the volume of sodium or potassium hydroxide 0,1 mol/l used for the sample, in ml;
1,4 is volumetric equivalent for nitrogen;
d is the dilution factor;
m is the mass of the sample, in grams.
The formula can be simplified as
(2)
where V B, V S, d and m have the same meaning as reported above.
10 Test report
The test report shall contain at least the following information:

a) a ll information necessary for the complete identification of the sample;
b) t est method used with reference to this European Standarddocument, including its
year of publication, i.e. EN 15562EN 15562:2023;
c) t est results obtained expressed as percentage mass fraction of total nitrogen in the
fertilizer;
d) d
ate of sampling and sampling procedure (if known);
e) d
ate when the analysis was finished;
f) a ll operating details not specified in this document, or regarded as optional, together
with details of any incidents that occurred when performing the method which might
have inf luenced the test result(s).

Bibliography
E N 1482‑1, Fertilizers and liming materials — Sampling and sample preparation —
[1]
Part 1: Sampling
[2]
Regulation (EC) No 2003/2003 of the European Parliament and of the Council of 13
October 2003 relating to fertilisers, Official Journal L 304, 21/11/2003, P. 0001-
0194, Annex IV, method 2.4

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BS EN 15562:2023
BSI Standards Publication
Inorganic fertilizers — Determination

of cyanamide nitrogen
BS EN 15562:2023 BRITISH STANDARD
National foreword
This British Standard is the UK implementation of EN 15562:2023. It
supersedes BS EN 15562:2009, which is withdrawn.
The UK participation in its preparation was entrusted to Technical
Committee CII/37, Fertilisers and related chemicals.
A list of organizations represented on this committee can be obtained on
request to its committee manager.
Contractual and legal considerations
This publication has been prepared in good faith, however no
representation, warranty, assurance or undertaking (express or
implied) is or will be made, and no responsibility or liability is or will be
accepted by BSI in relation to the adequacy, accuracy, completeness or
reasonableness of this publication. All and any such responsibility and
liability is expressly disclaimed to the full extent permitted by the law.
This publication is provided as is, and is to be used at the
recipient’s own risk.
The recipient is advised to consider seeking professional guidance with
respect to its use of this publication.
This publication is not intended to constitute a contract. Users are
responsible for its correct application.
ISBN 978 0 539 18858 5
ICS 65.080
Compliance with a British Standard cannot confer immunity from
legal obligations.
Standards Policy and Strategy Committee on 31 August 2023.

Date Text affected
BS EN 15562:2023
EUROPEAN STANDARD EN 15562

NORME EUROPÉENNE
EUROPÄISCHE NORM August 2023
ICS 65.080 Supersedes EN 15562:2009
English Version
Inorganic fertilizers - Determination of cyanamide

nitrogen
Engrais inorganiques - Dosage de l'azote cyanamidé Anorganische Düngemittel - Bestimmung des
Cyanamidstickstoffs
This European Standard was approved by CEN on 26 June 2023.
concerning such national standards may be obtained on application to the CEN-CENELEC 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
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, Türkiye and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION

COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2023 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 15562:2023 E
worldwide for CEN national Members.
BS EN 15562:2023
EN 15562:2023 (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
7 Sampling and sample preparation ................................................................................................. 5
8 Procedure ................................................................................................................................................ 6
8.1 Preparation of the solution for analysis ....................................................................................... 6
8.2 Analysis of the solution....................................................................................................................... 6
8.3 Blank test ................................................................................................................................................. 7
8.4 Control test .............................................................................................................................................. 7
9 Expression of the result ...................................................................................................................... 7
10 Test report............................................................................................................................................... 8
Bibliography ......................................................................................................................................................... 9
2
BS EN 15562:2023
EN 15562:2023 (E)
European foreword
This document (EN 15562:2023) has been prepared by Technical Committee CEN/TC 260 “Fertilizers
and liming materials”, the secretariat of which is held by DIN.
This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by February 2024, and conflicting national standards shall
be withdrawn at the latest by February 2024.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN 15562:2009.
In comparison with the previous edition EN 15562:2009, the following technical modifications have been
made:
— technical changes have been made to the description of the procedure (Clause 8) and to Table 1 (8.2);
— deletion of distillation apparatus drawings.
This document has been prepared under a standardization request addressed to CEN by the European
Commission. The Standing Committee of the EFTA States subsequently approves these requests for its
Member States.
Any feedback and questions on this document should be directed to the users’ national standards body.
A complete listing of these bodies can be found on the CEN website.
According to the CEN-CENELEC Internal Regulations, the national standards organisations of the
following countries are bound to implement this European Standard: 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, Türkiye and the United
Kingdom.
3
BS EN 15562:2023
EN 15562:2023 (E)
1 Scope
This document specifies a method for the determination of cyanamide nitrogen in fertilizers. The method
is applicable to calcium cyanamide and mixtures of calcium cyanamide with calcium nitrate.
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 — Vocabulary — Part 1: General terms
EN 12944-2, Fertilizers and liming materials — 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 terminology 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
Precipitation of cyanamide nitrogen as a silver complex. Digestion in sulfuric acid with the aid of a
catalyst. Distillation of the ammonia from an alkaline solution, absorption in an excess of sulfuric acid
volumetric solution and back-titration with sodium or potassium hydroxide volumetric solution.
5 Reagents
Use only reagents of recognized analytical grade and water with an electrical conductivity < 0,5 mS/m (at
25 °C).
5.1 Glacial acetic acid
5.2 Ammonia solution, containing 10 % of ammonia gas by mass, ρ20 = 0,96 g/ml
5.3 Ammoniacal silver solution, according to Tollens
Mix 500 ml of 10 % silver nitrate (AgNO3) solution in water with 500 ml of 10 % ammonia solution (5.2).
Do not expose unnecessarily to light, heat or air. The solution normally keeps for years. As long as the
solution remains clear, the reagent is of good quality.
5.4 Sulfuric acid, mass concentration ρ20 = 1,84 g/ml
5.5 Potassium sulphate, analytical grade
4
BS EN 15562:2023
EN 15562:2023 (E)
5.6 Catalyst
Use 0,3 g to 0,4 g of copper (II) oxide or 0,95 g to 1,25 g of copper (II) sulphate pentahydrate for each
determination.
5.7 Sulfuric acid, substance concentration c = 0,05 mol/l
5.8 Sodium or potassium hydroxide, substance concentration c = 0,1 mol/l, carbonate free
5.9 Indicator solutions
5.9.1 Mixed indicator
Solution A: Dissolve 0,1 g of methyl red in 3,7 ml of sodium or potassium hydroxide, c = 0,1 mol/l (5.8)
and make up to 100 ml with water.
Solution B: Dissolve 0,1 g of methylene blue in water and make up to 100 ml.
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.
5.9.2 Methyl red indicator
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 5.9.1.
5.10 Sodium hydroxide, 30 % m/v, mass concentration, ρ20 = 1,33 g/ml, ammonia free
5.11 Anti-bump granules of pumice stone, washed in hydrochloric acid and calcined
5.12 Potassium thiocyanate, (mass fraction wN = 14,4 %), analytical grade
6 Apparatus and equipment

Usual laboratory glassware and equipment and, in particular, the following.
6.1 Distillation apparatus, according to Kjeldahl, 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.
Automatic distillation apparatus may be used also, provided that the results are statistically equivalent.
6.2 Graduated flask, capacity 500 ml
6.3 Kjeldahl flask, long necked and of suitable capacity (300 ml to 500 ml)
6.4 Pipette, capacity 25 ml and 50 ml
6.5 Rotary shaker, 35 turns to 40 turns per minute
6.6 Graduated burette, 50 ml. (div. 1/10)
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.
5
BS EN 15562:2023
EN 15562:2023 (E)
Sample preparation shall be carried out in accordance with EN 1482-2.
8 Procedure
WARNING — When using any ammoniacal silver solution safety goggles shall be worn. As soon as a thin
membrane forms on the surface of the liquid, an explosion can be produced by agitation and the greatest
caution is essential.
8.1 Preparation of the solution for analysis
According to Table 1, weigh, to the nearest 0,001 g, the prescribed quantity of sample and place it in a
suitable glass mortar. Grind the sample three times with water, pouring off the water after each grinding
into a 500 ml graduated flask (6.2). Transfer quantitatively the sample into the 500 ml graduated flask
(6.2), washing the mortar, pestle and funnel with water. Make up with water to approximately 400 ml.
Add 15 ml of acetic acid (5.1). Shake on the rotary shaker (6.5) for approximately 2 h.
Make up to 500 ml with water, mix and filter.
The analysis shall be carried out as quickly as possible.
8.2 Analysis of the solution
According to Table 1, transfer with a pipette (6.4) the prescribed volume of the filtrate into a 250 ml
beaker.
Add ammonia solution (5.2) until slightly alkaline and add 30 ml of warm ammoniacal silver nitrate (5.3)
to precipitate the yellow silver complex of the cyanamide.
Leave overnight, filter and wash the precipitate with cold water until it is completely free of ammonia.
Place the filter and the precipitate, still moist, in a Kjeldahl flask (6.3), add 10 g to 15 g of potassium
sulphate (5.5), the appropriate amount of the catalyst (5.6), 50 ml of water and 25 ml of concentrated
sulfuric acid (5.4).
Warm the flask slowly, while shaking it gently until the contents come to the boil. Increase the heat, boil
until the contents of the flask become colourless or pale green.
Continue boiling for approximately 1 h, then leave to cool.
Slowly add 100 ml to 150 ml of water with a gentle swirling. Wait the solution to cool.
Using a graduated burette (6.6), place in the receiving flask 50 ml of sulfuric acid 0,05 mol/l (5.7). Add
the appropriate quantity of the chosen indicator (5.9.1 or 5.9.2) and, if necessary, water to get a volume
of at least 50 ml. The end of the extension tube of the condenser shall be below the surface of the solution.
Quantitatively transfer the digested solution into the distillation flask of the apparatus (6.1). Add water
to get a total volume of about 350 ml and several grains of pumice (5.11) to control the boiling.
Assemble the distillation apparatus (6.1) and, taking care to avoid any loss of ammonia, add to the
contents of the distillation flask 200 ml of 30 % m/v sodium hydroxide (5.10).
Gradually warm the flask, and when boiling begins, distil at the 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 the liquid.
Test the subsequent distillate by means of an appropriate reagent to ensure that all the ammonia is
completely distilled. Wash the condenser extension with water.
6
BS EN 15562:2023
EN 15562:2023 (E)
Titrate the excess of sulphuric acid (5.7) with the sodium or potassium hydroxide (5.8) using a graduated
burette (6.6), until the solution turns from purple to grey using the mixed indicator (5.9.1).
Table 1 — Weighing and dilution
Declaration N% Amount to be Dilution Solution of sample to be Dilution factor

weighed digested and distilled
g ml ml
0 to 5 10 500 50 10
5 to 10 10 500 25 20
10 to 20 5 500 25 20
8.3 Blank test
Carry out a blank test (omitting the sample) under the same conditions and refer to this in the calculation
of the final result.
8.4 Control test
Before carrying out the analysis, check that the apparatus is working properly and that the correct
technique is applied weighing, to the nearest 0,001 g, 5 g of potassium thiocyanate (5.12) and proceeding
as in 8.1 and 8.2.
9 Expression of the result

Calculate the content of cyanamide nitrogen as a percentage mass fraction of the fertilizer as received for
analysis according to Formula (1):
=N%
(VB − VS ) ⋅ 1, 4 ⋅ d ⋅ 100 (1)
m ⋅ 1000
where
VB is the volume of sodium or potassium hydroxide 0,1 mol/l used for the blank, in ml;
VS is the volume of sodium or potassium hydroxide 0,1 mol/l used for the sample, in ml;
1,4 is volumetric equivalent for nitrogen;
d is the dilution factor;
m is the mass of the sample, in grams.
The formula can be simplified as
N % =
(VB − VS ) ⋅ 0, 14 ⋅ d (2)
m
where VB, VS, d and m have the same meaning as reported above.
7
BS EN 15562:2023
EN 15562:2023 (E)
10 Test report
The test report shall contain at least the following information:
a) all information necessary for the complete identification of the sample;
b) test method used with reference to this document, including its year of publication, i.e.
EN 15562:2023;
c) test results obtained expressed as percentage mass fraction of total nitrogen in the fertilizer;
d) date of sampling and sampling procedure (if known);
e) date when the analysis was finished;
f) all operating details not specified in this document, or regarded as optional, together with details of
any incidents that occurred when performing the method which might have influenced the test
result(s).
8
BS EN 15562:2023
EN 15562:2023 (E)
Bibliography
[1] EN 1482-1, Fertilizers and liming materials — Sampling and sample preparation — Part 1: Sampling
9
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Inorganic fertilizers –—Emergency

IMPORTANT — PLEASE NOTE

Text example 1 — indicates added text (in green)

About Tracked Changes

© The British Standards Institution 2023

ISBN 978 0 539 28464 5

Amendments/corrigenda issued since publication

The UK participation in its preparation was entrusted to

A list of organizations represented on this committee can be

This publication does not purport to include all the necessary

Compliance with a British Standard cannot confer

This British Standard was published under the authority of the

Amendments/corrigenda issued since publication

Date Text affected

This document supersedes CEN/TS 15562:2007EN 15562:2009.

In comparison with the previous edition EN 15562:2009, the following technical

This document has been prepared under a mandate givenstandardization request

According to the CEN/-CENELEC Internal Regulations, the national standards

© BSI 2023 – All rights reserved vii

This European Standarddocument specifies a method for the determination of cyanamide

The following referenced documents are indispensable forreferred to in the applicationtext

EN 12944‑1:1999EN 12944‑1, Fertilizers and liming materials and soil improvers —

EN 12944‑2:1999, Fertilizers and liming materials and soil improvers — Vocabulary —

3 Terms and definitions

Precipitation of cyanamide nitrogen as a silver complex. Digestion in sulfuric acid with

© BSI 2023 – All rights reserved 1

5.25.1 Glacial acetic acid

5.35.2 Ammonia solution, containing 10 % of ammonia gas by mass (, ρ 20 = 0,96 g/ml).

5.45.3 Ammoniacal silver solution, according to Tollens.

5.55.4 Concentrated sulfuricSulfuric acid, mass concentration ρ 20 = 1,84 g/ml.

5.65.5 Potassium sulfatesulphate, p.a.analytical grade

5.8 Sodium hydroxide solution, approximately 30 % NaOH (ρ 20 = 1,33 g/ml), ammonia

5.95.7 Sulfuric acid, substance concentration c = 0,05 mol/l.

5.105.8 Sodium or potassium hydroxide solution,, substance concentration

5.115.9 Indicator solutions

5.11.15.9.1 Mixed indicator

Solution A: Dissolve 10,1 g of methyl red in 373,7 ml of sodium hydroxide solutionor

Mix one volume of solution A with two volumes of solution B.

2 © BSI 2023 – All rights reserved

5.11.25.9.2 Methyl red indicator solution

6 Apparatus and equipment

Usual laboratory glassware and equipment and, in particular, the following.

6.1 Distillation apparatus

Consisting Distillation apparatus, according to Kjeldahl, consisting of a round-bottomed

© BSI 2023 – All rights reserved 3

4 © BSI 2023 – All rights reserved

Figure 1 Distillation apparatus 1

© BSI 2023 – All rights reserved 5

Figure 2 Distillation apparatus 2

6 © BSI 2023 – All rights reserved

Figure 3 Distillation apparatus 3

© BSI 2023 – All rights reserved 7

4 500 ml flask for the collection of the distillate

Figure 4 Distillation apparatus 4

6.2 Graduated flask, capacity 500 ml.

6.4 Pipette, capacity 25 ml and 50 ml.

6.5 Rotary shaker, 35 turns to 40 turns per minute.