1、Fertilizers and liming materials Sampling of static heaps Technical report on experimental sampling trials performed under mandate M/454 PD CEN/TR 17040:2017 BSI Standards Publication WB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06National foreword This Published Document is the UK implemen
2、tation of CEN/TR 17040:2017. The UK participation in its preparation was entrusted to Technical Committee CII/37, Fertilisers and related chemicals. A list of organizations represented on this committee can be obtained on request to its secretary. This publication does not purport to include all the
3、 necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2017. Published by BSI Standards Limited 2017 ISBN 978 0 580 94470 3 ICS 65.080 Compliance with a British Standard cannot confer immunity from legal obligations. This Published D
4、ocument was published under the authority of the Standards Policy and Strategy Committee on 31 March 2017. Amendments/corrigenda issued since publication Date Text affected PUBLISHED DOCUMENT PD CEN/TR 17040:2017 TECHNICAL REPORT RAPPORT TECHNIQUE TECHNISCHER BERICHT CEN/TR 17040 February 2017 ICS 6
5、5.080 English Version Fertilizers and liming materials - Sampling of static heaps - Technical report on experimental sampling trials performed under mandate M/454 Engrais et amendements minraux basiques - chantillonnage des tas statiques - Compte-rendu technique des essais dechantillonnage raliss so
6、us le mandat M/454 Dngemittel und Kalkdnger - Probenahme aus statischen Haufwerken - Technischer Bericht ber Probenahmeversuche im Rahmen des Mandats M/454This 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 nati
7、onal 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, Ser
8、bia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2017 CEN All rights of exploitation in any form and by
9、 any means reserved worldwide for CEN national Members. Ref. No. CEN/TR 17040:2017 E PD CEN/TR 17040:2017CEN/TR 17040:2017 (E) 2 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 studie
10、s . 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 4.4 The 1 ste
11、xperimental trial (see A.1) . 12 4.5 The 2 ndexperimental trial (see A.2) 12 4.6 The 3 rdexperimental 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 pri
12、nciple 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 A.1 The 1 stexperimental trial . 17 A.1.1 General . 17 A.1.2 Description of the site 17 A.1.3 Constitution of the conical and recta
13、ngular 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 PD CEN/TR 17040:2017CEN/TR 17040:2017 (E) 3 A.1.6 Sampling of the rectangular heap . 21 A.1.7 Chemical analysis . 21 A.1.8 Granulometric an
14、alysis 21 A.1.9 Conclusions of the 1 sttrial . 21 A.2 The 2 ndexperimental 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
15、 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 A.2.9 Conclusions of the 2 ndtrial 27 A.3 The 3 rdexperimental trial . 29 A.3.1 General . 29 A.3.2 Description of the site . 29 A.3.3 Constitution of the
16、 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
17、 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 PD CEN/TR 17040:2017CEN/TR 17040:2017 (E) 4 C.4 Nobbe spear
18、. 39 C.5 Double tube spear 39 C.6 Test of manual spears . 39 C.7 Consideration 41 Bibliography . 42 PD CEN/TR 17040:2017CEN/TR 17040:2017 (E) 5 European foreword This document (CEN/TR 17040:2017) has been prepared by Technical Committee CEN/TC 260 “Fertilizers and liming materials”, the secretariat
19、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
20、 Commission and the European Free Trade Association. PD CEN/TR 17040:2017CEN/TR 17040:2017 (E) 6 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 t
21、he 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 con
22、trol 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 St
23、ates 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 sa
24、mpling 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
25、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 downstr
26、eam 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.
27、 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
28、 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”. PD CEN/T
29、R 17040:2017CEN/TR 17040:2017 (E) 7 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 ferti
30、lizer 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
31、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 an
32、d 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.
33、EU Member States official fertilizer controls are required to check the nutrient contents and the composition of fertilizers placed on the market. The purpose of Regulation (EC) No2003/2003 1 is to guarantee the farmer the quality of the fertilizer. The first step of the fertilizers control is the s
34、ampling 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 effo
35、rt 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 developm
36、ent 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 Inter
37、national 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 t
38、he accuracy of the elaborated sampling method as compared with the sampling in motion of the same fertilizer according to EN 1482-1; PD CEN/TR 17040:2017CEN/TR 17040:2017 (E) 8 d) determine which size of static fertilizer heap could be sampled using existing sampling instruments, and which fertilize
39、r 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 whic
40、h 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
41、” 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. After the presentation of the results of the 1 stand the 2 ndtrial CEN/TC 260/WG 1 de
42、cided to perform the 3 rdand last trial on a liming material product. 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 El
43、evator 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 cases of the 1 sta
44、nd the 2 ndexperimental trials. This transfer was not performed in the case of the 3 rdtrial because of: heaps transfer from storage cell to another isnt usual for liming materials, the plant doesnt lend itself to this transfer. 4.2.2 Mass of the heap to be sampled The final mass of the static conic
45、al heap was 430 t for the 1 stexperimental trial and was reduced to 250 t for the 2 ndand 3 rdtrial 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 samplin
46、g were performed: 1) sampling in the flow, and 2) sampling from the static conical heaps, 3) sampling from the rectangular heap (1 stan 2 ndexperimental trials). PD CEN/TR 17040:2017CEN/TR 17040:2017 (E) 9 4.2.3.2 Sampling in the flow (product in motion) Independent sampling in the flow was performe
47、d 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 specifie
48、d 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
49、 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 fertilizers 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. PD CEN/TR 17040:2017CEN/TR 17040:2017
