SIST-TP CEN/TR 17040:2017

SLOVENSKI STANDARD
SIST-TP CEN/TR 17040:2017
01-december-2017
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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
SIST-TP CEN/TR 17040:2017 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST-TP CEN/TR 17040:2017


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.

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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
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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
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C.4 Nobbe spear . 39
C.5 Double tube spear . 39
C.6 Test of manual spears . 39
C.7 Consideration . 41
Bibliography . 42

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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.
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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”.
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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;
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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).
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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.
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Step 1

Step 2

Step 3

Step 4
Figure 1 — Distribution of the sample units on the intermediate cones (top view)
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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.
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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
...