Fertilizers - Crushing strength determination on fertilizers grains

This Technical Report is applicable to crushing strength measurement as applied to grains of fertilizers obtained in prilling or wet-granulation process. Compacted or crystalline materials were not considered.

Düngemittel - Bestimmung der Kornfestigkeit auf Düngemittelkörnern

Engrais - Détermination de la résistance à l'écrasement des engrais

Le présent document porte sur la mesure de la résistance à l’écrasement appliquée aux grains d’engrais obtenus par les process de prilling ou de granulation humide. Les matériaux compactés ou cristallins n’ont pas été pris en compte.

Gnojila - Določanje odpornosti granul gnojil proti drobljenju

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
18-Aug-2021
Due Date
23-Oct-2021
Completion Date
08-Oct-2021

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Standards Content (sample)

SLOVENSKI STANDARD
SIST-TP CEN/TR 12333:2021
01-november-2021
Nadomešča:
SIST CR 12333:1999
Gnojila - Določanje odpornosti granul gnojil proti drobljenju
Fertilizers - Crushing strength determination on fertilizers grains
Düngemittel - Bestimmung der Kornfestigkeit auf Düngemittelkörnern
Engrais - Détermination de la résistance à l'écrasement des engrais
Ta slovenski standard je istoveten z: CEN/TR 12333:2021
ICS:
65.080 Gnojila Fertilizers
SIST-TP CEN/TR 12333:2021 en

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

---------------------- Page: 1 ----------------------
SIST-TP CEN/TR 12333:2021
---------------------- Page: 2 ----------------------
SIST-TP CEN/TR 12333:2021
CEN/TR 12333
TECHNICAL REPORT
RAPPORT TECHNIQUE
June 2021
TECHNISCHER BERICHT
ICS 65.080 Supersedes CR 12333:1996
English Version
Fertilizers - Crushing strength determination on fertilizers
grains

Engrais - Détermination de la résistance à l'écrasement Düngemittel - Bestimmung der Kornfestigkeit auf

des engrais Düngemittelkörnern

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 12333:2021 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST-TP CEN/TR 12333:2021
CEN/TR 12333:2021 (E)
Contents Page

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

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

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

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

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

4 Principle ........................................................................................................................................................... 5

5 Apparatus ........................................................................................................................................................ 5

6 Sample preparation ..................................................................................................................................... 6

7 Procedure ........................................................................................................................................................ 6

8 Test report ....................................................................................................................................................... 6

9 Statistical calculations ................................................................................................................................ 7

10 Expression of results ................................................................................................................................... 7

11 Conclusion ....................................................................................................................................................... 8

Annex A (informative) Flow chart of statistical calculations ..................................................................... 9

Annex B (informative) Crushing strength — Interlaboratory test........................................................ 10

Annex C (informative) Crushing strength — Interlaboratory test — Outlier deleted ................... 11

Annex D (informative) Crushing strength — Interlaboratory test — Outlier deleted ................... 12

Annex E (informative) Crushing strength — Interlaboratory test — No outlier in this

grouping ........................................................................................................................................................ 13

Annex F (informative) Crushing strength — Interlaboratory test — Outlier deleted ................... 14

Bibliography .............................................................................................................................................................. 15

---------------------- Page: 4 ----------------------
SIST-TP CEN/TR 12333:2021
CEN/TR 12333:2021 (E)
European foreword

This document (CEN/TR 12333:2021) 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 12333:1996.
Significant changes between this document and CR 12333:1996 are as follows:

a) 24/8/8, 13/13/21 and 0/10/20 changed to NPK 24+8+8, NPK 13+13+21 and PK 10+20,

respectively;
b) adaption to current principles and rules for structure and drafting.

The present report arises from work done by CEN/TC 260/WG 2 under the work item “Crushing strength

determination” with the view of producing a European Standard.

Unfortunately, after several ring tests, results appeared to be so randomly distributed that a statistically

significant interpretation showing good reproducibility and repeatability could not be obtained.

Tests on correlation have also shown that no significant correlation as to the causes of the dispersion of

the results could be obtained within the proposed time scale and probably not without expending too

much effort, time and money.

Therefore, since the results obtained may be added to those of past publications in the literature,

CEN/TC 260 decided the results obtained should not be ignored by the scientific community.

---------------------- Page: 5 ----------------------
SIST-TP CEN/TR 12333:2021
CEN/TR 12333:2021 (E)
Introduction

The resistance to crushing (crushing strength) of fertilizer is an important property used in quality

control of fertilizer production. It influences the storage and handling as well as spreading properties of

fertilizer.

However, crushing strength of fertilizer grains is not a constant property stricto sensu. Crushing strength

is significantly influenced by the content of free water in the fertilizer, humidifying and drying during

storage, as well as by temperature changes. Time dependent processes in the grain and bulk during the

lifetime of the grains may also affect the crushing strength.

Nevertheless, there are several “in house” methods used for the measurement of crushing strength of

fertilizer grains which give different results. There is also a need for a standardized method.

This document reports the results of the international ring test, organized by CEN/TC 260/WG 2

(physical properties), carried out 1992, with the purpose of standardizing the measurement technique of

crushing strength.
---------------------- Page: 6 ----------------------
SIST-TP CEN/TR 12333:2021
CEN/TR 12333:2021 (E)
1 Scope

This document is applicable to crushing strength measurement as applied to grains of fertilizer obtained

in prilling or wet-granulation process. Compacted or crystalline materials were not considered.

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.

ISO 565:1990, Test sieves — Metal wire cloth, perforated metal plate and electroformed sheet — Nominal

sizes of openings

ISO 5725:1986, Precision of test methods — Determination of repeatability and reproducibility for a

standard test method by inter-laboratory tests
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

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/
3.1
crushing strength of grains
force necessary to destroy the grain as such
4 Principle

The measurement of the force applied for the destruction of the grains may be carried out by constant

load or constant speed.

NOTE Not all manufacturers of apparatus can give information about the principle (constant speed or constant

load) used.

It is not known which of the first “peak” or maximum of force applicable on the grain is measured.

The grains undergoing the measurement were of the same size.
5 Apparatus
5.1 Sieves

The sieve is in accordance with ISO 565:1990 for the grain size chosen. In this ring test, the grain size was

2,8 mm (retained in the mesh of the sieve).

ISO 5725:1986 has been withdrawn and replaced by the ISO 5725 (series) released between 1994 and 1998.

---------------------- Page: 7 ----------------------
SIST-TP CEN/TR 12333:2021
CEN/TR 12333:2021 (E)
5.2 Crushing strength measuring apparatus
In this ring test, the following apparatus as given in Table 1 were used:
Table 1
Compression speed
mm/min Direction
low high
Alvetron 10 vertical
Dinamometro Ceast 5, 10, 20 vertical
Erweka THB 28 8 38, 48, 55 horizontal
Forcemeter 10 vertical
lnstrou 4502 10 55 vertical
Matec Accuforce II 10 vertical
Mecmesin 10 55 vertical
Salter EFG-2 10 55 vertical

To investigate the influence of compression speed and/or direction of the crushing force applied, in this

ring test both low and/or high compression speed were allowed in both directions: horizontally and

vertically.
6 Sample preparation

The ring test included products with high and low elasticity. The following products or formulations have

been chosen:
Urea; AN; NPK 24+8+8; NPK 13+13+21; PK 10+20.

The test was taken with 5 × 25 = 125 grains of each formula. The grain size was d = 2,8 mm (in order to

be retained in the mesh of the sieve).
To carry ou
...

SLOVENSKI STANDARD
kSIST-TP FprCEN/TR 12333:2021
01-marec-2021
Gnojila - Določanje odpornosti granul gnojil proti drobljenju
Fertilizers - Crushing strength determination on fertilizers grains
Düngemittel - Bestimmung der Kornfestigkeit auf Düngemittelkörnern
Engrais - Détermination de la résistance à l'écrasement des engrais
Ta slovenski standard je istoveten z: FprCEN/TR 12333
ICS:
65.080 Gnojila Fertilizers
kSIST-TP FprCEN/TR 12333:2021 en,fr,de

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

---------------------- Page: 1 ----------------------
kSIST-TP FprCEN/TR 12333:2021
---------------------- Page: 2 ----------------------
kSIST-TP FprCEN/TR 12333:2021
FINAL DRAFT
TECHNICAL REPORT
FprCEN/TR 12333
RAPPORT TECHNIQUE
TECHNISCHER BERICHT
January 2021
ICS Will supersede CR 12333:1996
English Version
Fertilizers - Crushing strength determination on fertilizers
grains

Engrais - Détermination de la résistance à l'écrasement Düngemittel - Bestimmung der Kornfestigkeit auf

des engrais Düngemittelkörnern

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 12333:2021 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
kSIST-TP FprCEN/TR 12333:2021
FprCEN/TR 12333:2021 (E)
Contents Page

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

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

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

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

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

4 Principle ........................................................................................................................................................... 5

5 Apparatus ........................................................................................................................................................ 5

6 Sample preparation ..................................................................................................................................... 6

7 Procedure ........................................................................................................................................................ 6

8 Test report ....................................................................................................................................................... 6

9 Statistical calculations ................................................................................................................................ 7

10 Expression of results ................................................................................................................................... 7

11 Conclusion ....................................................................................................................................................... 8

Annex A (informative) Flow chart of statistical calculations ..................................................................... 9

Annex B (informative) Crushing strength — Interlaboratory test........................................................ 10

Annex C (informative) Crushing strength — Interlaboratory test — Outlier deleted ................... 11

Annex D (informative) Crushing strength — Interlaboratory test — Outlier deleted ................... 12

Annex E (informative) Crushing strength — Interlaboratory test — No outlier in this

grouping ........................................................................................................................................................ 13

Annex F (informative) Crushing strength — Interlaboratory test — Outlier deleted ................... 14

Bibliography .............................................................................................................................................................. 15

---------------------- Page: 4 ----------------------
kSIST-TP FprCEN/TR 12333:2021
FprCEN/TR 12333:2021 (E)
European foreword

This document (FprCEN/TR 12333:2021) 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.
This document will supersede CR 12333:1996.

The present report arises from work done by CEN/TC 260/WG 2 under the work item “Crushing strength

determination” with the view of producing a European Standard.

Unfortunately, after several ring tests, results appeared to be so randomly distributed that a statistically

significant interpretation showing good reproducibility and repeatability could not be obtained.

Tests on correlation have also shown that no significant correlation as to the causes of the dispersion of

the results could be obtained within the proposed time scale and probably not without expending too

much effort, time and money.

Therefore, since the results obtained may be added to those of past publications in the literature,

CEN/TC 260 decided the results obtained should not be ignored by the scientific community.

Significant changes between this document and CR 12333:1996 are as follows:

a) 24/8/8, 13/13/21 and 0/10/20 changed to NPK 24+8+8, NPK 13+13+21 and PK 10+20,

respectively;
b) adaption to current principles and rules for structure and drafting.
---------------------- Page: 5 ----------------------
kSIST-TP FprCEN/TR 12333:2021
FprCEN/TR 12333:2021 (E)
Introduction

The resistance to crushing (crushing strength) of fertilizer is an important property used in quality

control of fertilizer production. It influences the storage, handling as well as spreading properties of

fertilizer.

However, crushing strength of fertilizer grains is not a constant property stricto sensu. Crushing strength

is significantly influenced by the content of free water in the fertilizer, humidifying and drying during

storage as well as by temperature changes. Time dependent processes in the grain and bulk during the

lifetime of the grains may also affect the crushing strength.

Nevertheless, there are several “in house” methods used for the measurement of crushing strength of

fertilizer grains which give different results. There is also a need for a standardized method.

This document reports the results of the international ring test, organized by CEN/TC 260/WG 2

(physical properties), carried out 1992, with the purpose of standardizing the measurement technique of

crushing strength.
---------------------- Page: 6 ----------------------
kSIST-TP FprCEN/TR 12333:2021
FprCEN/TR 12333:2021 (E)
1 Scope

This document is applicable to crushing strength measurement as applied to grains of fertilizer obtained

in prilling or wet-granulation process. Compacted or crystalline materials were not considered.

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.

ISO 565:1990, Test sieves — Metal wire cloth, perforated metal plate and electroformed sheet — Nominal

sizes of openings

ISO 5725:1986, Precision of test methods — Determination of repeatability and reproducibility for a

standard test method by inter-laboratory tests
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

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/
3.1
crushing strength of grains
force necessary to destroy the grain as such
4 Principle

The measurement of the force applied for the destruction of the grains may be carried out by constant

load or constant speed.

NOTE Not all manufacturers of apparatus can give an information about the principle (constant speed or

constant load) used.

It is not known which of the first “peak” or maximum of force applicable on the grain is measured.

The grains undergoing the measurement were of the same size.
5 Apparatus
5.1 Sieves

The sieve is in accordance with ISO 565:1990 for the grain size chosen. In this ring test, the grain size was

2,8 mm (retained in the mesh of the sieve).
---------------------- Page: 7 ----------------------
kSIST-TP FprCEN/TR 12333:2021
FprCEN/TR 12333:2021 (E)
5.2 Crushing strength measuring apparatus
In this ring test, the following apparatus as given in Table 1 were used:
Table 1
Compression speed
mm/min Direction
low high
Alvetron 10 vertical
Dinamometro Ceast 5, 10, 20 vertical
Erweka THB 28 8 38, 48, 55 horizontal
Forcemeter 10 vertical
lnstrou 4502 10 55 vertical
Matec Accuforce II 10 vertical
Mecmesin 10 55 vertical
Salter EFG-2 10 55 vertical

To investigate the influence of compression speed and/or direction of the crushing force applied, in this

ring test both low and/or high compression speed were allowed in both directions: horizontally and

vertically.
6 Sample preparation

The ring test included products with high and low elasticity. The following products or formulations have

been chosen:
Urea; AN; NPK 24+8+8; NPK 13+13+21; PK 10+20.

The test was taken with 5 × 25 = 125 grains of each formula. The grain size was d = 2,

...

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