CEN/TR 17040:2017
(Main)Fertilizers and liming materials - Sampling of static heaps - Technical report on experimental sampling trials performed under mandate M/454
Fertilizers and liming materials - Sampling of static heaps - Technical report on experimental sampling trials performed under mandate M/454
This document covers reports on three experimental sampling studies which have been performed under mandate M/454 in order to check the accuracy of the developed sampling method for sampling of static heaps by comparing it to the sampling of the same fertilizer product in motion according to EN 1482-1 and to determine which sizes of static fertilizer heap, if any, can be sampled using existing sampling equipment.
Düngemittel und Kalkdünger - Probenahme aus statischen Haufwerken - Technischer Bericht über Probenahmeversuche im Rahmen des Mandats M/454
Engrais et amendements minéraux basiques - Échantillonnage des tas statiques - Compte-rendu technique des essais d'echantillonnage réalisés sous le mandat M/454
Le présent document couvre les rapports de trois études expérimentales d'échantillonnage qui ont été effectuées dans le cadre du mandat M/454 de manière à vérifier l'exactitude de la méthode développée pour l'échantillonnage des tas statiques en la comparant à l'échantillonnage du même engrais en mouvement conformément à l'EN 1482-1 et à déterminer quelles tailles de tas d'engrais statique peuvent, si possible, être échantillonnées en utilisant les équipements d'échantillonnage existants.
Gnojila in sredstva za apnjenje - Vzorčenje statičnih kupov - Tehnično poročilo o postopkih eksperimentalnega vzorčenja v okviru mandata M/454
To tehnično poročilo zajema tehnični opis eksperimentalnega dela za pripravo metod vzorčenja gnojil in sredstev za apnjenje iz statičnih kupov.
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
01-december-2017
*QRMLODLQVUHGVWYD]DDSQMHQMH9]RUþHQMHVWDWLþQLKNXSRY7HKQLþQRSRURþLORR
SRVWRSNLKHNVSHULPHQWDOQHJDY]RUþHQMDYRNYLUXPDQGDWD0
Fertilizers and liming materials - Sampling of static heaps - Technical report on
experimental sampling trials performed under mandate M/454
Düngemittel und Kalkdünger - Probenahme aus statischen Haufwerken - Technischer
Bericht über Probenahmeversuche im Rahmen des Mandats M/454
Engrais et amendements minéraux basiques - Échantillonnage des tas statiques -
Compte-rendu technique des essais d'echantillonnage réalisés sous le mandat M/454
Ta slovenski standard je istoveten z: CEN/TR 17040:2017
ICS:
65.080 Gnojila Fertilizers
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
CEN/TR 17040
TECHNICAL REPORT
RAPPORT TECHNIQUE
February 2017
TECHNISCHER BERICHT
ICS 65.080
English Version
Fertilizers and liming materials - Sampling of static heaps -
Technical report on experimental sampling trials
performed under mandate M/454
Engrais et amendements minéraux basiques - Düngemittel und Kalkdünger - Probenahme aus
Échantillonnage des tas statiques - Compte-rendu statischen Haufwerken - Technischer Bericht über
technique des essais d'echantillonnage réalisés sous le Probenahmeversuche im Rahmen des Mandats M/454
mandat M/454
This Technical Report was approved by CEN on 2 January 2017. 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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, 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: Avenue Marnix 17, B-1000 Brussels
© 2017 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TR 17040:2017 E
worldwide for CEN national Members.
Contents Page
European foreword . 5
Introduction . 6
1 Scope . 7
2 Normative references . 7
3 Background . 7
3.1 General . 7
3.2 Requested tasks . 7
4 Experimental sampling studies . 8
4.1 General . 8
4.2 Sampling protocol . 8
4.2.1 Protocol . 8
4.2.2 Mass of the heap to be sampled . 8
4.2.3 Types of sampling . 8
4.3 Sampling instruments . 11
4.3.1 General . 11
4.3.2 Suitable instruments for granulated fertilizers . 11
4.3.3 Suitable instruments for liming materials . 11
st
4.4 The 1 experimental trial (see A.1) . 12
nd
4.5 The 2 experimental trial (see A.2) . 12
rd
4.6 The 3 experimental trial (see A.3) . 12
5 Development of sampling protocols . 12
5.1 Simulation of sampling protocols . 12
5.2 Statistical analysis . 13
5.3 Discussion and conclusions . 13
5.3.1 General . 13
5.3.2 Basic principle of sampling . 13
5.3.3 Segregation . 14
5.4 Scope of the experimental trials . 15
6 Conclusions . 15
Annex A (informative) Reports about the experimental trials . 17
st
A.1 The 1 experimental trial . 17
A.1.1 General . 17
A.1.2 Description of the site . 17
A.1.3 Constitution of the conical and rectangular heaps . 17
A.1.3.1 General . 17
A.1.3.2 Conical heap . 17
A.1.3.3 Rectangular heap . 18
A.1.4 Sampling in the flow . 18
A.1.5 Sampling of the conical heap. 19
A.1.6 Sampling of the rectangular heap . 21
A.1.7 Chemical analysis . 21
A.1.8 Granulometric analysis . 21
st
A.1.9 Conclusions of the 1 trial . 21
nd
A.2 The 2 experimental trial . 23
A.2.1 General . 23
A.2.2 Description of the site . 23
A.2.3 Constitution of the conical and rectangular heaps . 23
A.2.3.1 General . 23
A.2.3.2 Conical heap . 23
A.2.3.3 Rectangular heap . 24
A.2.4 Sampling in the flow . 24
A.2.5 Sampling of the conical heap . 25
A.2.6 Sampling of the rectangular heap . 26
A.2.7 Chemical analysis . 27
A.2.8 Granulometric analysis . 27
nd
trial . 27
A.2.9 Conclusions of the 2
rd
A.3 The 3 experimental trial . 29
A.3.1 General . 29
A.3.2 Description of the site . 29
A.3.3 Constitution of the conical heap . 30
A.3.4 Sample division . 30
A.3.5 Sampling in the flow . 30
A.3.6 Sampling of the conical heap . 31
A.3.7 Chemical analysis . 33
A.3.8 Granulometric analysis . 33
A.3.9 Conclusions of the comparative analyses . 34
Annex B (informative) Literature review . 36
B.1 Introduction. 36
B.2 Inventory of standards . 36
B.3 Inventory of best practice guidelines . 36
B.4 Inventory of legislation . 37
Annex C (informative) Sampling instruments - Equipment for static heap sampling . 39
C.1 General . 39
C.2 Manual spears . 39
C.3 Monotube spear. 39
C.4 Nobbe spear . 39
C.5 Double tube spear . 39
C.6 Test of manual spears . 39
C.7 Consideration . 41
Bibliography . 42
European foreword
This document (CEN/TR 17040:2017) 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 has been prepared under a mandate given to CEN by the European Commission and the
European Free Trade Association.
Introduction
With mandate M/454 of October 2009 the EC asked the European Committee for Standardization (CEN)
for a second extension to the standardization mandate M/335 concerning the modernization of the
methods of analysis of fertilizers.
This extension concerns the framework of Regulation (EC) No 2003/2003 relating to fertilizers and
liming materials [1].
The establishment of European Standards for methods of sampling and analysis is of utmost importance
to guarantee a uniform application and control of the European legislation in all member states.
Standardized methods of sampling and analysis are an indispensable element in guaranteeing a high
level of quality and safety of EC fertilizers for the benefit of purchasers.
In order to avoid any improper use of the term EC-fertilizer Member States are required to check the
compliance of such fertilizers or liming materials with the Regulation. To do this effectively,
representative sampling is a prerequisite for reliable analytical results.
Within the framework of mandate M/335, CEN/TC 260 developed EN 1482-1 which applies only to the
sampling of bulk material while it is being moved i.e. when any part of the fertilizer has an equal chance
of being part of the incremental sample, and EN 1482-2 which specifies the sample preparation. In
March 2009, a meeting of the Fertilizers Working Group of the EC took place to better define the current
sampling practices in the different Member States. Two Member States recommended further
improvements of EN 1482-1 as regards the sampling of static heaps.
Further enforcement authorities have limited resources for conformity assessment, and these are most
efficiently deployed at the downstream end of the supply chain, i.e. at retailer or farmers premises.
Therefore, nutrient content compliance should be ideally controlled at the point of sale to the end user,
i.e. at the end of the supply chain. The fertilizer or liming material may be delivered or stored at this
point in a bulk heap. Therefore EN 1482-1 might not fully satisfy the needs of Member States and an
evaluation should be carried out by CEN to see whether a representative sample can be obtained from
bulk heaps and if so what size of fertilizer heaps could be sampled at affordable costs.
Therefore mandate M/454 from the EC asked the European Committee for Standardization (CEN) to
provide standardized methods for sampling static heaps.
In resolution BT C093/2009, the CEN Technical Board (BT) accepted mandate M/454 and allocated the
work to CEN/TC 260, more specifically to its working group WG 1 “Sampling”.
1 Scope
This document covers reports on three experimental sampling studies which have been performed
under mandate M/454 in order to check the accuracy of the developed sampling method for sampling
of static heaps by comparing it to the sampling of the same fertilizer product in motion according to
EN 1482-1 and to determine which sizes of static fertilizer heap, if any, can be sampled using existing
sampling equipment.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
EN 1482-1:2007, Fertilizers and liming materials — Sampling and sample preparation — Part 1:
Sampling
EN 1482-3, Fertilizers and liming materials — Sampling and sample preparation — Part 3: Sampling of
static heaps
3 Background
3.1 General
Both producers and traders of fertilizers and liming materials have to guarantee a high level of quality
in the nutrient amount and physical parameters of fertilizers they put on the market. EU Member State’s
official fertilizer controls are required to check the nutrient contents and the composition of fertilizers
placed on the market. The purpose of Regulation (EC) No°2003/2003 [1] is to guarantee the farmer the
quality of the fertilizer.
The first step of the fertilizer’s control is the sampling in order to deliver a representative sample of a
fertilizer placed on the market. Any bias during the sampling could lead to great economical and/or
environmental consequences.
Sampling according to EN 1482-1 requires that a static heap has to be put in motion and this requires
time and effort to be spent by the sampling officials. Official control authorities cannot always be
present when static heaps are being formed or loaded for transport.
Consequently, the EC asked CEN/TC 260 “Fertilizers and liming materials” with Mandate M/454 for
investigation of the possibility of the development of a European Standard and, if appropriate, to
develop such a standard giving a sampling method of static fertilizer heaps for official controls that
guarantees reliable analytical results.
3.2 Requested tasks
The following main tasks were requested:
a) Monitoring the literature as well as International and European Standards in similar fields and an
evaluation of their relevance to this project (see Annex B);
b) elaboration and technical description of a method protocol to sample static heaps;
c) organization, performance and evaluation of experimental sampling studies in order to check the
accuracy of the elaborated sampling method as compared with the sampling in motion of the same
fertilizer according to EN 1482-1;
d) determine which size of static fertilizer heap could be sampled using existing sampling
instruments, and which fertilizer types could be covered by the scope of the new sampling method.
4 Experimental sampling studies
4.1 General
The objective of the experimental sampling studies was to check if it is possible to take samples from
static heaps of fertilizers which have an equivalent representativeness to samples which have been
taken from the product in motion in accordance with EN 1482-1.
Basically it was proposed to undertake three comparative experimental trials using three mineral
fertilizer types with chemical and granulometric characteristics more and more heterogeneous as
follows:
1) Granulated “straight” fertilizer → 2) granulated “complex” NPK fertilizer → 3) “blend” NPK fertilizer.
The experimental trials were undertaken in collaboration with industrial partners in their facilities in
order to be closer to reality.
st nd
After the presentation of the results of the 1 and the 2 trial CEN/TC 260/WG 1 decided to perform
rd
and last trial on a liming material product.
the 3
4.2 Sampling protocol
4.2.1 Protocol
The same protocol was followed during each of the three trials. Firstly a static conical heap was built up
in 4 steps using the transport chain of the storage plant as follows:
Receiving pit → Elevator → Several conveyor belts → Discharging in the storage cell onto the heap.
Secondly the conical heap was transferred to an adjacent storage cell with a loader on wheels so as to
form a static rectangular heap. The constitution of this static rectangular heap was performed in the
st nd rd
cases of the 1 and the 2 experimental trials. This transfer was not performed in the case of the 3
trial because of:
— heap’s transfer from storage cell to another isn’t usual for liming materials,
— the plant doesn’t lend itself to this transfer.
4.2.2 Mass of the heap to be sampled
st
The final mass of the static conical heap was 430 t for the 1 experimental trial and was reduced to
nd rd
250 t for the 2 and 3 trial according to the advice of the CEN/TC 260/WG 1 after consideration of the
results of the first trial.
4.2.3 Types of sampling
4.2.3.1 General
During the building up of the heap, three types of sampling were performed:
1) sampling in the flow, and
2) sampling from the static conical heaps,
st nd
3) sampling from the rectangular heap (1 an 2 experimental trials).
4.2.3.2 Sampling in the flow (product in motion)
Independent sampling in the flow was performed according to EN 1482-1 as follows:
— use of a stream sampling cup as described in EN 1482-1:2007, 5.4.2;
— sampling of the increments in the fall of the product;
— random sampling during the whole period of the product downloading;
— the number of sampling points was always higher than the number specified in EN 1482-1, in
Regulation (EC) No 2003/2003 [1] and according to CEN/TC 260/WG 1;
— the total mass of the aggregate samples was always higher than 4 kg.
4.2.3.3 Sampling of the static conical heaps
Sampling from each static conical heap was performed following the specific protocol developed for the
project. For each intermediate cone, the number of sample units was defined beforehand. These sample
units were then distributed on the surface of each intermediate cone (see Figure 1), the arrow
representing the conveyor belt and the direction of the fertilizer’s flow. Taking into account the actual
size of the cone, the geometrical dimensions of the sample units were calculated so that they represent
an equal quantity of fertilizer. The calculation takes into account the previous cone.
Step 1
Step 2
Step 3
Step 4
Figure 1 — Distribution of the sample units on the intermediate cones (top view)
The sampling of the conical heap was conducted according to the sampling protocol:
— use of a spear with double tube (granulated fertilizer) or a tube shovel (wet liming material), see
4.3;
— sampling at the sampling points in each sample unit as pre-defined, the sample units represent
equal quantities of fertilizer;
— random sampling in the sample units;
— taking 8 to 10 sampling points per sample unit so as to obtain a total mass of max. 4 kg per sample
unit.
4.2.3.4 Sampling of the static rectangular heaps
The rectangular heap was sampled according to Regulation (EC) No 2003/2003 [1]. The surface of the
heap was subdivided into sample units by drawing an imaginary grid such that each grid area
represented an equal quantity of fertilizer. The number of grid areas exceeded the number of
incremental samples required and each represented a sample unit.
In each sample unit, one increment was sampled in a random way using a spear with double tube. This
st nd
procedure was performed within the 1 and the 2 experimental trial (granulated fertilizer).
4.3 Sampling instruments
4.3.1 General
The equipment depends on the product (particle size and flow ability) and on the mass of samples
required. The equipment has to be neutral (no influence on the sample like impurities or crushing) and
should be easily cleaned to avoid contaminations between samples. For manual sampling the use of a
spear makes it possible to work at some different depths inside the bulk.
Different types of manual and automatic spears and other types of equipment have been tested for their
suitability to sample static heaps of fertilizers and liming materials. It was found that the spears with a
double tube are the most used and adapted for sampling in bulk because they are more solid and easier
to use. Spears should be used both in a vertically and horizontally way in order to take samples in
different shapes of bulk.
4.3.2 Suitable instruments for granulated fertilizers
For granulated fertilizers the spear with double tubes and multiple openings was identified as the most
appropriate sampling instrument: robust, simple to use, easily transportable (for one person) and not
very expensive. During sampling of the static heap, it was possible to reach a depth of at most 1 m using
this spear. In practice, it is difficult to go deeper than 0,9 m depending on the operator's force.
4.3.3 Suitable instruments for liming materials
For wet liming materials a tube shovel, which is a kind of shovel with a handle, the plate of the shovel
being a tube, was identified to be the most appropriate sampling instrument, because the nature of the
material means that only a very small amount would enter the openings in the double tube instrument.
In the tube shovel the tube is about 30 cm long and has a large diameter of 12 cm to 13 cm. There is no
closing system at the entrance. The sampling is done into the surface of the heap. This sampling
instrument is a good compromise. It easily penetrates the material (± 30 cm deep), and avoids any bias
in the sampling caused by the falling down of particles in the sample (closed system). As the liming
material is quite compact the sample stays in the tube.
st
4.4 The 1 experimental trial (see A.1)
® ®
The experimental trial No I was performed with a granulated “straight” fertilizer: YaraBela SULFAN
th th
24+18. This trial took place in the storage plant of YARA in Aunay-Sous-Crécy (France) from 4 to 7
June 2012. For the detailed description, results and conclusions see A.1.
nd
4.5 The 2 experimental trial (see A.2)
The experimental trial No II was performed with a granulated “complex” NPK fertilizer: SECOFlex 13-6-
th th
23 + SO (12). This trial took place in the storage plant of Leseur SA in Carhaix (France) from 24 to 26
June 2013. For the detailed description, results and conclusions see A.2.
rd
4.6 The 3 experimental trial (see A.3)
The experimental trial No III was performed with a liming material: wet chalk (particle size of 0 mm to
12 mm), 80 % passing at 2 mm sieve. The trial took place in the production and storage plant of
th th
GROUPE MEAC SAS in Villeau (France) from 05 to 07 February 2014. For the detailed description,
results and conclusions see A.3.
5 Development of sampling protocols
5.1 Simulation of sampling protocols
The complex procedure of sampling which was developed within the framework of the project aims at:
— generating a reference for the comparative analyses for each parameter (chemical
content/characteristics and particle size distribution) with the average of the results of the
4 representative samples taken from the fertilizer/liming material flow according to EN 1482-1;
— generating a cartography in three dimensions of the conical heap with the chemical and
granulometric characteristics of the fertilizer/liming material;
— being able to simulate different protocols of representative sampling in the conical heap and to
compare their results with the reference;
— being able to study the influence of the size of the conical heap on the representativeness of the
studied protocols of sampling.
The objective being the determination of the best protocol for sampling the static heap, five simulations
of sampling the conical heap were developed as follows:
— The complete sampling: this simulation has to be considered as an ideal sampling plan in the
conical heap. Indeed, the “sampler” takes as many samples as the number of units of sampling
defined in the conical heap.
— The partial sampling around the base of the cone: this simulation can be considered as a classic
sampling in the conical heap. The “sampler” takes samples around the base of the cone.
— The partial sampling by following an edge of the cone: this simulation takes samples from the
conical heap by rising from the base up to the top. The “sampler” takes 2 to 4 samples according to
the size of the cone (2 or 4 layers, 2 or 4 sample units).
— The reduced random sampling (5 samples): this simulation takes samples from the conical heap in
a random way. The “sampler” takes 5 representative samples distributed in a random way over the
whole heap.
— The widened random sampling (10 samples): This simulation takes samples from the conical heap
in a random way. The “sampler” takes 10 representative samples distributed in a random way over
the whole heap.
The five simulations have been applied to the intermediate conical heaps corresponding to the four
constitutive steps of the formation of the conical heap so as to highlight any possible influence of the
size of the static conical heap.
5.2 Statistical analysis
The objective was to determine the best protocol of sampling the conical heap. This protocol has to
supply a result equivalent to the reference sampling taken from the flow during the formation of the
cone according to EN 1482-1.
On the basis of samples taken from the conical heaps, the various protocols of sampling (complete,
partial, random etc.) of the cones were simulated and their results were compared with the reference
constituted by the granulometric (D16, D84, GSI…) and chemical (main nutrients, Neutralizing Value for
the liming material) analyses of samples taken from the flow (according to EN 1482-1) during the four
constitutive steps.
The statistical analysis bases itself on a multiple comparison of averages, which allows determination of
any significant differences between the series of observations. It is, however, necessary to verify the
relevance of these differences from a practical and/or regulatory point of view.
5.3 Discussion and conclusions
5.3.1 General
The project’s partners asked CEN/TC 260/WG 1 to take into account the following considerations for
the elaboration of a standard method for sampling of static heaps.
5.3.2 Basic principle of sampling
The basic principle for sampling fertilizer is that each particle has the same chance of becoming part of
the sample. In practice, it is not possible to apply this basic principle in the sampling of a static conical
heap. We can consider only the upper layer of the heap as being the sampling zone (see Figure 2).
Figure 2 — Sampling of a static heap using a spear
The depth from which a sample can be obtained is dependent on the length of the sampling device and
the nature of the product being sampled. During the trials, a spear (double tubes and multiple openings)
for granulated fertilizers and a tube shovel for the liming material have been used. It was demonstrated
that it is physically impossible to drive the spear/tube shovel into the heap more than 0,9 m but to at
most 1 m deep in the granulated fertilizer and 0,30 m in the liming material.
Consequently, the sampling zone of the static conical heap is the upper layer of the heap having a
thickness of at most 1 m for granulated fertilizers and 0,30 m for liming materials.
It has, therefore, to be recognized that the principle for sampling a static heap is that each particle of the
upper layer has the same chance of becoming part of the sample. In this way it can be considered that
the upper layer is representative of the whole static heap.
5.3.3 Segregation
During trials, segregation has been observed during the building up of the heap, even where the
fertilizer is well homogeneous (e.g. trial I). Segregation is a natural process which occurs when the
fertilizer is transported or piled onto a heap. Large granules rise to the top of the load during the
transport and roll to the bottom during heaping (see Figure 3).
Figure 3 — Segregation during the building up of the static heap
Segregation is caused by the granulometric characteristics of the product and affects the granulometric
distribution of the particles in the heap. The more the granulometric distribution of the fertilizer is
extended, the more the particles will be segregated in the heap. Consequently, if the nutrient content is
a function of the granulometry (e.g. in the case of blended fertilizers), the nutrient distribution inside
the conical heap is also affected by the segregation.
The aim of the project was to determine a sampling protocol which mitigates the effects of the
segregation and reconstitutes the initial mixing of particles.
As mentioned above, the segregation phenomenon has been observed during all trials, but was more
pronounced during the last trial with the liming material. This is the result of the use of a less
homogeneous product. However the granulometric parameters of the samples taken from the heaps
have been affected by segregation much more strongly than the chemical parameters of the samples,
provided that the products were granulated (straight or complex) or chemically very homogenous
(liming material) independent of the granulometry.
Because of the segregation the effect of heap's size has also been observed. The sample units are defined
on the surface area of the heap. The greater the heap the larger the surface area and smaller the area of
each sampling unit which represents the same mass. Consequently there are more sampling units the
greater the heap. Therefore the influence of one sample unit has a lower impact on the result of the
sampling when the heap is greater.
5.4 Scope of the experimental trials
The initial scope of the experimental trials covered more and more heterogeneous (chemically and
st
granulometrically) products as: granulated straight fertilizers (1 trial), granulated complex fertilizers
nd rd
(2 trial) and blend complex fertilizers (3 trial).
However, a wide discussion was conducted between the CEN/TC 260/WG 1 experts during the 12th
meeting (January 2013) and the 13th meeting (December 2013) about the opportunity to conduct the
rd
3 trial with a blended fertilizer since these products are not stored typically in large static heaps.
Normally blended fertilizers are delivered directly to the user in small quantities or stored in big-bags
for a short time. Therefore, the question was raised whether another heterogeneous product, a static
rd
heap of which is more likely to occur in practice should be selected for the 3 trial.
Therefore, it was proposed to select a liming material as these products are very often sampled in
practice from static heaps and may be heterogeneous. Moreover liming materials have been covered by
the EU-Fertilizers Legislation since 2013 and it will be essential that these products are covered by the
scope of EN 1482-3 as they are covered also by EN 1482-1 and EN 1482-2.
It was, therefore agreed by the CEN/TC 260/WG 1 experts that the scope of the experimental trials and
their conclusions should cover a single nutrient granulated fertilizer, a uniform complex granulated
fertilizer and a milled or granulated liming material.
6 Conclusions
The partial sampling around the base of the heap does not supply a representative sample because of
the phenomenon of size segregation. During the formation of the fertilizer heap, bigger diameter
particles run down to the base of the heap while the fine particles concentrate on the top of the heap.
This phenomenon generated significant differences between the described sampling protocol and the
reference.
Under the conditions of the experimental trials and for the fertilizer types tested (granulated “straight”
or “complex” fertilizers and liming materials), it is possible to realize:
— a partial sampling constituted by at least 40 to 50 increments (= sampling points) taken along an
edge by rising from the base to the top of the heap, or,
— a partial sampling constituted by at least 40 to 50 increments (= sampling points) taken randomly
from the whole surface of the heap.
The results of chemical analyses of the samples obtained following these protocols will not be
statistically different from the inflow reference samples (EN 1482-1). The results of the granulometric
analyses of the samples obtained following these protocols were not statistically different from the
inflow reference samples (EN 1482-1) for the two kinds of granulated fertilizers (granulated “straight”
or “complex” fertilizer) but not for the liming material due to the high segregation propensity of this
product.
st nd
Within the 1 and 2 experimental trial, the conical heaps were transferred to another storage cell with
a loader on wheels so as to form a static rectangular heap. This rectangular was sampled according to
Regulation (EC) No 2003/2003 [1].
The samples taken in the flow according to EN 1482-1 from the conical heap and from the rectangular
heap have been re-mixed so as to provide three representative samples of the fertilizer lot provided by
three different ways of sampling. These samples were analyzed (chemical and granulometric analysis)
and the results were reported. Although there are some differences, on a practical point of view and
regarding the measurement uncertainty, it can be considered that the results are similar. However, a
statistical study has not been conducted since it was not within the purpose of the trial.
Annex A
(informative)
Reports about the experimental trials
st
A.1 The 1 experimental trial
A.1.1 General
The first comparative test was realized in association with the industrial partner YARA in the storage
site of Aunay-Sous-Crécy (France). The product used during this first trial was a granulated nitrogenous
® ®
sulfured “straight fertilizer” (YaraBela SULFAN 24+18) chosen for its chemical and granulometric
homogeneity.
A.1.2 Description of the site
The plant is classified Seveso, comprised of two main storage buildings with a total storage capacity of
30 000 t. This site is equipped with a weighing machine for the trucks. The hall 1 (called “HR1”, with a
capacity of 15 000 t) was chosen for the trial due to the fact that it is equipped with a conveyor and is
subdivided into cells.
A.1.3 Constitution of the conical and rectangular heaps
A.1.3.1 General
The constitution of the conical and rectangular heaps was a complex operation. The total mass of
fertilizer was 430 t and was transported by 17 trucks with an average capacity of 25,4 t. The conical
heap was transferred to an adjacent cell with a wheel loader to form the rectangular heap. The
execution of these two steps was possible due to the collaboration and support of YARA and the
employees of this storage plant.
A.1.3.2 Conical heap
The constitution of the conical heap was conducted in four steps and needed two days. For each step,
the dimensions of the conical heap were measured (see Table A.1). At the end, the conical heap had a
height of 4,37 m, an average diameter of 18 m and a total mass of 431,44 t. The height of the cone has
been measured with a laser pointed on the top of the conical heap. The diameter of the heap was
measured with a target drawn beforehand on the floor.
Table A.1 — Characteristics of the conical heap for each step of its constitution
Steps 1 2 3 4
Downloading time (hh:mm:ss) 00:05:26 00:29:29 01:28:55 03:02:23
Downloading speed (t/h) 99,8 86,9 85,2 83,4
Added quantity (t) 9,04 42,70 126,30 253,40
Height of the cone (m) 1,20 2,19 3,17 4,37
Radius of the cone(m) 2,50 4,48 6,70 9,00
Added volume (m ) 7,85 38,14 103,02 219,11
The objective of the step by step constitution of the conical heap is to establish a comparison between
the sampling procedure (in the flow or in the heap) for increasing lot sizes.
A.1.3.3 Rectangular heap
The conical heap was transferred into an adjacent cell using a loader on wheels and formed into a
rectangular heap which had the following approximated size: height of 2,25 m, width of 13,5 m, length
of 23,5 m and the same total mass of 430 t.
This transfer aims at comparing the classical sampling procedure for rectangular heaps with the
sampling in the flow and in the conical heap.
A.1.4 Sampli
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