Straight ammonium nitrate fertilizers - Comparative study on the determination of porosity (oil retention)

This CEN report gives the results of inter-laboratory testing to compare the accuracy and convenience of the official EC method for porosity measurement (given as Annex B) with two non-standardized alternative methods (given as Annexes C and D) already used in some participating laboratories.

Reine Ammoniumnitratdünger - Bestimmung der Porosität (Ölretention)

Engrais simples à base de nitrate d'ammonium - Etude comparative de méthodes de détermination de la porosité (rétention fuel)

Le présent document fournit les résultats de l’essai interlaboratoires servant à comparer la précision et la praticité de la méthode CE officielle pour la mesure de la porosité (décrite dans l’Annexe B) avec deux méthodes alternatives non normalisées (décrites dans les Annexes C et D) déjà utilisées par certains laboratoires participants.
Trois produits, ayant une porosité comprise entre 1 % et 7 %, ont été utilisés pour les essais interlaboratoires.

Čista amonnitratna gnojila - Primerjalna študija o določanju poroznosti (zadrževanje olja)

General Information

Status
Published
Public Enquiry End Date
01-Apr-2021
Publication Date
07-Oct-2021
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
13-Jul-2021
Due Date
17-Sep-2021
Completion Date
08-Oct-2021

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SLOVENSKI STANDARD
SIST-TP CEN/TR 14539:2021
01-november-2021
Nadomešča:
SIST-TR CR 14539:2003
Čista amonnitratna gnojila - Primerjalna študija o določanju poroznosti
(zadrževanje olja)

Straight ammonium nitrate fertilizers - Comparative study on the determination of

porosity (oil retention)
Reine Ammoniumnitratdünger - Bestimmung der Porosität (Ölretention)
Engrais simples à base de nitrate d'ammonium - Etude comparative de méthodes de
détermination de la porosité (rétention fuel)
Ta slovenski standard je istoveten z: CEN/TR 14539:2021
ICS:
65.080 Gnojila Fertilizers
SIST-TP CEN/TR 14539:2021 en

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

---------------------- Page: 1 ----------------------
SIST-TP CEN/TR 14539:2021
---------------------- Page: 2 ----------------------
SIST-TP CEN/TR 14539:2021
CEN/TR 14539
TECHNICAL REPORT
RAPPORT TECHNIQUE
June 2021
TECHNISCHER BERICHT
ICS 65.080 Supersedes CR 14539:2002
English Version
Straight ammonium nitrate fertilizers - Comparative study
on the determination of porosity (oil retention)

Engrais simples à base de nitrate d'ammonium - Etude Reine Ammoniumnitratdünger - Bestimmung der

comparative de méthodes de détermination de la Porosität (Ölretention)
porosité (rétention fuel)

This Technical Report was approved by CEN on 23 May 2021. It has been drawn up by the Technical Committee CEN/TC 260.

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.
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. CEN/TR 14539:2021 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST-TP CEN/TR 14539:2021
CEN/TR 14539:2021 (E)
Contents Page

European foreword ............................................................................................................................................ 3

Introduction .......................................................................................................................................................... 4

1 Scope .......................................................................................................................................................... 5

2 Normative references .......................................................................................................................... 5

3 Terms and definitions ......................................................................................................................... 5

4 Test procedure ....................................................................................................................................... 5

4.1 Methods for measuring porosity ..................................................................................................... 5

4.2 Products ................................................................................................................................................... 5

4.2.1 Test samples: straight ammonium nitrate .................................................................................. 5

4.2.2 Gas oils ...................................................................................................................................................... 6

4.3 Ring test procedure .............................................................................................................................. 6

5 Results and statistical interpretation ............................................................................................ 6

5.1 General...................................................................................................................................................... 6

5.2 Mean value .............................................................................................................................................. 6

5.3 Repeatability .......................................................................................................................................... 7

5.4 Reproducibility ...................................................................................................................................... 7

5.5 Interpretation of the results ............................................................................................................. 7

6 Conclusions ............................................................................................................................................. 7

Annex A (informative) Characteristics of and limits for straight ammonium nitrate fertilizers

of high nitrogen content as given in EC Directive 80/876/EEC ............................................ 8

Annex B (informative) Determination of oil retention — EC method as given in EC Directive

87/94/EEC ............................................................................................................................................... 9

Annex C (informative) Centrifuge method — Non-standardized alternative method ............ 12

Annex D (informative) Roller drum method — Non-standardized alternative method ........ 15

Bibliography ....................................................................................................................................................... 18

---------------------- Page: 4 ----------------------
SIST-TP CEN/TR 14539:2021
CEN/TR 14539:2021 (E)
European foreword

This document (CEN/TR 14539:2021) has been prepared by Technical Committee CEN/TC 260

“Fertilizers and liming materials”, the secretariat of which is held by DIN.

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 CR 14539:2002.
Significant changes between this document and CR 14539:2002 are as follows:
a) updated Normative references and Bibliography;
b) adaption to current principles and rules for structure and drafting.

This document is published for information only and does not have the status of a European Standard.

The Annexes A to D are informative.
---------------------- Page: 5 ----------------------
SIST-TP CEN/TR 14539:2021
CEN/TR 14539:2021 (E)
Introduction

Straight ammonium nitrate fertilizers of high nitrogen content (> 28 %), following Directive

80/876/EEC [1] and Directive 87/94/EEC [2], are subject to the particular regulatory requirement of a

maximum porosity limit of 4 %. The currently used official EC method is demanding with respect to time

and skilled laboratory manpower.

Therefore, this document presents a comparison of non-standardized alternative methods for measuring

porosity with the official one, through ring testing.
In parallel, oil retention can also be determined using ISO 5313 [4].
---------------------- Page: 6 ----------------------
SIST-TP CEN/TR 14539:2021
CEN/TR 14539:2021 (E)
1 Scope

This document gives the results of inter-laboratory testing to compare the accuracy and convenience of

the official EC method for porosity measurement (given in Annex B) with two non-standardized

alternative methods (given in Annexes C and D) already used in some participating laboratories.

Three products, with a porosity between 1 % and 7 %, have been used in the inter-laboratory trials.

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 1235, Solid fertilizers - Test sieving (ISO 8397)
3 Terms and definitions
No terms and definitions are listed in this document.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https://www.iso.org/obp
— IEC Electropedia: available at https://www.electropedia.org/
4 Test procedure
4.1 Methods for measuring porosity

All the methods tested for measurement of ammonium nitrate porosity are based on immersion of the

test sample in gas oil, removing the excess oil, and finally determining the absorbed amount of oil through

weighing. The methods differ in the way of removing the excess oil.
Table 1 — Methods for measuring porosity
Method Removal of oil Protocol
Method 1: EC Method [2] Hand-rubbing between sheets of filter paper see Annex B
Method 2: Centrifuge method Draining and centrifuging see Annex C

Method 3: Roller drum method Draining and roller drum with filter thimble see Annex D

This method is based on ISO 5313 [4], with some minor but significant differences.

WARNING — Appropriate safety rules and procedures should be followed while handling samples and

residues of Ammonium nitrate impregnated with gas oil.
4.2 Products
4.2.1 Test samples: straight ammonium nitrate

Three different ammonium nitrate samples have been provided to all the participants. Two samples were

fertilizer ammonium nitrates of the 33,5 % N type, the third was a special ammonium nitrate, with a

higher porosity well over 4 %.
---------------------- Page: 7 ----------------------
SIST-TP CEN/TR 14539:2021
CEN/TR 14539:2021 (E)
4.2.2 Gas oils

All gas oils used in the ring test conformed to the requirements of Directive 87/94/EEC, Annex II [2]. In

order to improve the accuracy of the ring test, one specific gas oil, distributed centrally in this ring test,

has been used as a reference by all participants, parallel to oils from local origin.

4.3 Ring test procedure

This ring test has been performed by 17 participating laboratories, private ones as well as official ones.

Three ammonium nitrate samples have been tested by three different methods, using a reference gas oil,

and oils of local origin.

In order to avoid the influence of thermal cycling under different circumstances, test samples were

prepared centrally without further thermal cycling by the participating laboratories.

The participating laboratories were requested to perform at least two independent replicates of each

sample, according to each method.

Test results, observations and remarks have been reported on the appropriate sheets.

5 Results and statistical interpretation
5.1 General

Statistical calculations have been run on all the results, according to ISO 5725-2 [5] and ISO 3534-1 [3].

Repeatability and reproducibility have been evaluated for each sample coupled with each method.

Evaluations of the mean result have been carried out through variance analysis.
5.2 Mean value

Mean values for a given method have been evaluated, incorporating the influence of different gas oils and

the intra-laboratory variance.
See Table 2.
Table 2 — Mean values
Sample number
Method according to
Table 1
1 2 3
Method 1 2,20 6,22 1,42
Method 2 2,22 6,10 1,51
Method 3 1,89 6,28 1,42
---------------------- Page: 8 ----------------------
SIST-TP CEN/TR 14539:2021
CEN/TR 14539:2021 (E)
5.3 Repeatability

Table 3 gives the general evaluation of standard deviation with respect to repeatability for each couple

method/sample after checking the equality of variances using Bartlett’s test.
Table 3 — Repeatability
Sample number
Method according to
Table 1
1 2 3
Method 1 0,17 0,20 0,07
Method 2 0,12 0,15 0,06
Method 3 0,10 0,17 0,05
5.4 Reproducibility

Table 4 gives the general evaluation of standard deviation with respect to reproducibility for each couple

method/sample after checking the equality of variances using Bartlett’s test.
Table 4 — Reproducibility
Sample number
Method according to
Table 1
1 2 3
Method 1 0,64 0,73 0,14
Method 2 0,75 0,64 0,28
Method 3 0,47 0,66 0,11
5.5 Interpretation of the results

When the typology of mean results is examined, the statistical proof of the existence of two groups

corresponding to the gas oil type can only be obtained in the case of the couple sample 1/method 1.

The comparison of the mean values obtained by the three methods in all cases, studied by variance

analysis of intra-laboratory means for each test shows that the methods are equivalent.

6 Conclusions

Based upon the above mentioned statistical tests, no significant difference between the methods can be

found; hence the accuracy of the different methods is equivalent.

From a practical point of view, the tested non-standardized alternative methods are more user-friendly

and more convenient than the official EC method.

It could not be shown that there is a statistical difference between results obtained with the different gas

oils conforming to the requirements of Directive 87/94/EEC, Annex II [2].
---------------------- Page: 9 ----------------------
SIST-TP CEN/TR 14539:2021
CEN/TR 14539:2021 (E)
Annex A
(informative)
Characteristics of and limits for straight ammonium nitrate fertilizers of
high nitrogen content as given in EC Directive 80/876/EEC
A.1 Porosity (oil retention)

The oil retention of the fertilizer, which shall first have undergone two thermal cycles of a temperature

ranging from 25 °C to 50 °C, shall not exceed 4 % by mass.
A.2 Combustible ingredients

The mass fraction of combustible material in per cent measured as carbon shall not exceed 0,2 % for

fertilizers having a nitrogen content of at least 31,5 % (mass fraction) and shall not exceed 0,4 % for

fertilizers having a nitrogen content of at least 28 % but less than 31,5 % (mass fraction).

A.3 pH

A solution of 10 g of fertilizer in 100 ml of water shall have a pH value of at least 4,5.

A.4 Particle size analysis

Not more than a mass fraction of 5 % of the fertilizer shall pass through a 1-mm mesh sieve and not more

than a mass fraction of 3 % shall pass through a 0,5-mm mesh sieve.
A.5 Chlorine
The maximum chlorine content is set at 0,02 % (mass fraction).
A.6 Heavy metals

Heavy metals should not be added deliberately, and any traces which are incidental to the production

process should not exceed the limit fixed by the Committee.
The mass fraction of copper shall not be higher than 10 mg/kg.
No limits are specified for other heavy metals.
---------------------- Page: 10 ----------------------
SIST-TP CEN/TR 14539:2021
CEN/TR 14539:2021 (E)
Annex B
(informative)
Determination of oil retention — EC method as given in EC Directive
87/94/EEC
B.1 General

This Annex specifies the procedure for the determination of oil retention of straight ammonium nitrate

fertilizers of high nitrogen content.

The method is applicable to both prilled and granular fertilizers which do not contain oil-soluble

materials.
B.2 Terms and definitions
For the purposes of this Annex, the following term and definition apply.
B.2.1
oil retention of a fertilizer

quantity of oil retained by the fertilizer determined under the operating conditions specified

Note 1 to entry: The oil retention is expressed as percentage by mass.
B.3 Principl
...

SLOVENSKI STANDARD
kSIST-TP FprCEN/TR 14539:2021
01-marec-2021
Čista amonnitratna gnojila - Primerjalna študija o določanju poroznosti
(zadrževanje olja)

Straight ammonium nitrate fertilizers - Comparative study on the determination of

porosity (oil retention)
Reine Ammoniumnitratdünger - Bestimmung der Porosität (Ölretention)
Engrais simples à base de nitrate d'ammonium - Etude comparative de méthodes de
détermination de la porosité (rétention fuel)
Ta slovenski standard je istoveten z: FprCEN/TR 14539
ICS:
65.080 Gnojila Fertilizers
kSIST-TP FprCEN/TR 14539:2021 en,fr,de

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

---------------------- Page: 1 ----------------------
kSIST-TP FprCEN/TR 14539:2021
---------------------- Page: 2 ----------------------
kSIST-TP FprCEN/TR 14539:2021
FINAL DRAFT
TECHNICAL REPORT
FprCEN/TR 14539
RAPPORT TECHNIQUE
TECHNISCHER BERICHT
January 2021
ICS Will supersede CR 14539:2002
English Version
Straight ammonium nitrate fertilizers - Comparative study
on the determination of porosity (oil retention)

Engrais simples à base de nitrate d'ammonium - Etude Reine Ammoniumnitratdünger - Bestimmung der

comparative de méthodes de détermination de la Porosität (Ölretention)
porosité (rétention fuel)

This draft Technical Report is submitted to CEN members for Vote. It has been drawn up by the Technical Committee CEN/TC

260.

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 Technical Report. It is distributed for review and comments. It is subject to change without

notice and shall not be referred to as a Technical Report.
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. FprCEN/TR 14539:2021 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
kSIST-TP FprCEN/TR 14539:2021
FprCEN/TR 14539:2021 (E)
Contents Page

European foreword ............................................................................................................................................ 3

Introduction .......................................................................................................................................................... 4

1 Scope .......................................................................................................................................................... 5

2 Normative references .......................................................................................................................... 5

3 Terms and definitions ......................................................................................................................... 5

4 Test procedure ....................................................................................................................................... 5

4.1 Methods for measuring porosity ..................................................................................................... 5

4.2 Products ................................................................................................................................................... 5

4.2.1 Test samples: straight ammonium nitrate .................................................................................. 5

4.2.2 Gas oils ...................................................................................................................................................... 6

4.3 Ring test procedure .............................................................................................................................. 6

5 Results and statistical interpretation ............................................................................................ 6

5.1 General...................................................................................................................................................... 6

5.2 Mean value .............................................................................................................................................. 6

5.3 Repeatability .......................................................................................................................................... 7

5.4 Reproducibility ...................................................................................................................................... 7

5.5 Interpretation of the results ............................................................................................................. 7

6 Conclusions ............................................................................................................................................. 7

Annex A (informative) Characteristics of and limits for straight ammonium nitrate fertilizers

of high nitrogen content as given in EC Directive 80/876/EEC ............................................ 8

Annex B (informative) Determination of oil retention — EC method as given in EC Directive

87/94/EEC ............................................................................................................................................... 9

Annex C (informative) Centrifuge method — Non-standardized alternative method ............ 12

Annex D (informative) Roller drum method — Non-standardized alternative method ........ 15

Bibliography ....................................................................................................................................................... 18

---------------------- Page: 4 ----------------------
kSIST-TP FprCEN/TR 14539:2021
FprCEN/TR 14539:2021 (E)
European foreword

This document (FprCEN/TR 14539:2021) 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 Vote on TR.

It is published for information only and does not have the status of a European Standard.

The Annexes A to D are informative.
This document will supersede CR 14539:2002.
Significant changes between this document and CR 14539:2002 are as follows:
a) updated normative references and bibliography;
b) adaption to current principles and rules for structure and drafting.
---------------------- Page: 5 ----------------------
kSIST-TP FprCEN/TR 14539:2021
FprCEN/TR 14539:2021 (E)
Introduction

Straight ammonium nitrate fertilizers of high nitrogen content (>28 %), following Directive

80/876/EEC [1] and Directive 87/94/EEC [2], are subject to the particular regulatory requirement of a

maximum porosity limit of 4 %. The currently used official EC method is demanding with respect to time

and skilled laboratory manpower.

Therefore, this document presents a comparison of non-standardized alternative methods for measuring

porosity with the official one, through ring testing.
Parallelly, oil retention can also be determined by ISO 5313.
---------------------- Page: 6 ----------------------
kSIST-TP FprCEN/TR 14539:2021
FprCEN/TR 14539:2021 (E)
1 Scope

This document gives the results of inter-laboratory testing to compare the accuracy and convenience of

the official EC method for porosity measurement (given as Annex B) with two non-standardized

alternative methods (given as Annexes C and D) already used in some participating laboratories.

Three products, with a porosity between 1 % and 7 %, have been used in the inter-laboratory trials.

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 1235, Solid fertilizers - Test sieving (ISO 8397:1988 modified)
3 Terms and definitions
No terms and definitions are listed in this document.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https://www.iso.org/obp
— IEC Electropedia: available at http://www.electropedia.org/
4 Test procedure
4.1 Methods for measuring porosity

All the methods tested for measurement of ammonium nitrate porosity are based on immersion of the

test sample in gas oil, removing the excess of oil, and finally determining the absorbed amount of oil

through weighing. The methods differ in the way of removing the excess oil.
Table 1 — Methods for measuring porosity
Method Removal of oil Protocol
Method 1: EC Method [2] Hand-rubbing between sheets of filter paper see Annex B
Method 2: Centrifuge method Draining and centrifuging see Annex C

Method 3: Roller drum method Draining and roller drum with filter thimble see Annex D

This method is based on ISO 5313, with some minor but significant differences.

WARNING — Appropriate safety rules and procedures should be followed while handling samples and

residues of Ammonium nitrate impregnated with gas oil.
4.2 Products
4.2.1 Test samples: straight ammonium nitrate

Three different ammonium nitrate samples have been provided to all the participants. Two samples were

fertilizer ammonium nitrates of the 33,5 % N type, the third was a special ammonium nitrate, with a

higher porosity well over 4 %.
---------------------- Page: 7 ----------------------
kSIST-TP FprCEN/TR 14539:2021
FprCEN/TR 14539:2021 (E)
4.2.2 Gas oils

All gas oils used in the ring test conformed to the requirements of Directive 87/94/EEC, Annex II [2]. In

order to improve the accuracy of the ring test, one specific gas oil, distributed centrally in this ring test,

has been used as a reference by all participants, parallel to oils from local origin.

4.3 Ring test procedure

This ring test has been performed by 17 participating laboratories, private ones as well as official ones.

Three ammonium nitrate samples have been tested by three different methods, using a reference gas oil,

and oils of local origin.

In order to avoid the influence of thermal cycling under different circumstances, test samples were

prepared centrally without further thermal cycling by the participating laboratories.

The participating laboratories were requested to perform at least two independent replicates of each

sample, according to each method.

Test results, observations and remarks have been reported on the appropriate sheets.

5 Results and statistical interpretation
5.1 General

Statistical calculations have been run on all the results, according to ISO 5725-2 and ISO 3534-1.

Repeatability and reproducibility have been evaluated for each sample coupled with each method.

Evaluations of the mean result have been carried out through variance analysis.
5.2 Mean value

Mean values for a given method have been evaluated, incorporating the influence of different gas oils and

the intra-laboratory variance.
See Table 2.
Table 2 — Mean values
Sample number
Method according to
Table 1
1 2 3
Method 1 2,20 6,22 1,42
Method 2 2,22 6,10 1,51
Method 3 1,89 6,28 1,42
---------------------- Page: 8 ----------------------
kSIST-TP FprCEN/TR 14539:2021
FprCEN/TR 14539:2021 (E)
5.3 Repeatability

Table 3 gives the general evaluation of standard deviation with respect to repeatability for each couple

method/sample after checking the equality of variances using Bartlett’s test.
Table 3 — Repeatability
Sample number
Method according to
Table 1
1 2 3
Method 1 0,17 0,20 0,07
Method 2 0,12 0,15 0,06
Method 3 0,10 0,17 0,05
5.4 Reproducibility

Table 4 gives the general evaluation of standard deviation with respect to reproducibility for each couple

method/sample after checking the equality of variances using Bartlett’s test.
Table 4 — Reproducibility
Sample number
Method according to
Table 1
1 2 3
Method 1 0,64 0,73 0,14
Method 2 0,75 0,64 0,28
Method 3 0,47 0,66 0,11
5.5 Interpretation of the results

When the typology of mean results is examined, the statistical proof of the existence of two groups

corresponding to the gas oil type can only be obtained in the case of the couple sample 1/method 1.

The comparison of the mean values obtained by the three methods in all cases, studied by variance

analysis of intra-laboratory means for each test shows that the methods are equivalent.

6 Conclusions

Based upon the above mentioned statistical tests, no significant difference between the methods can be

found; hence the accuracy of the different methods is equivalent.

From a practical point of view, the tested non-standardized alternative methods are more user-friendly

and more convenient than the official EC method.

It could not be shown that there is a statistical difference between results obtained with the different gas

oils conforming to the requirements of Directive 87/94/EEC, Annex II [2].
---------------------- Page: 9 ----------------------
kSIST-TP FprCEN/TR 14539:2021
FprCEN/TR 14539:2021 (E)
Annex A
(informative)
Characteristics of and limits for straight ammonium nitrate fertilizers of
high nitrogen content as given in EC Directive 80/876/EEC
A.1 Porosity (oil retention)

The oil retention of the fertilizer, which shall first have undergone two thermal cycles of a temperature

ranging from 25 °C to 50 °C, shall not exceed 4 % by mass.
A.2 Combustible ingredients

The mass fraction of combustible material in per cent measured as carbon shall not exceed 0,2 % for

fertilizers having a nitrogen content of at least 31,5 % (mass fraction) and shall not exceed 0,4 % for

fertilizers having a nitrogen content of at least 28 % but less than 31,5 % (mass fraction).

A.3 pH

A solution of 10 g of fertilizer in 100 ml of water shall have a pH value of at least 4,5.

A.4 Particle size analysis

Not more than a mass fraction of 5 % of the fertilizer shall pass through a 1-mm mesh sieve and not more

than a mass fraction of 3 % shall pass through a 0,5-mm mesh sieve.
A.5 Chlorine
The maximum chlorine content is set at 0,02 % (mass fraction).
A.6 Heavy metals

Heavy metals should not be added deliberately, and any traces which are incidental to the production

process should not exceed the limit fixed by the Committee.
The mass fraction of copper shall not be higher than 10 mg/kg.
No limits are specified for other heavy metals.
---------------------- Page: 10 ----------------------
kSIST-TP FprCEN/TR 14539:2021
FprCEN/TR 14539:2021 (E)
Annex B
(informative)
Determination of oil retention — EC method as given in EC Directive
87/94/EEC
B.1 General

This annex specifies the procedure for the determination of oil retention of straight ammonium nitrate

fertilizers of high nitrogen content.

The method is applicable to both prilled and granular fertilizers which do not contain oil-soluble

materials.
B.2 Terms and definitions
For the purposes of this annex, the following term and definition apply.
B.2.1
oil retention of a fertilizer
quantity of oil retained by the fertilizer determined under the operating con
...

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