BS EN 1482-3:2016 Incorporating February 2017 BS ENcorrigendum 1482-3:2016 BSI Standards Publication Fertilizers and liming materials — Sampling and sample preparation Part 3: Sampling of static heaps BS EN 1482-3:2016 BRITISH STANDARD National foreword This British Standard is the UK implementation of EN 1482-3:2016 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 necessary provisions of a contract Users are responsible for its correct application © The British Standards Institution 2017 Published by BSI Standards Limited 2017 ISBN 978 580 97505 ICS 65.080 Compliance with a British Standard cannot confer immunity from legal obligations This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 August 2016 Amendments/corrigenda issued since publication Date Text affected 28 February 2017 Implementation of CEN/CENELEC Correction Notice 17 August 2016: Figure replaced BS EN 1482-3:2016 EN 1482-3 EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM August 2016 ICS 65.080 English Version Fertilizers and liming materials - Sampling and sample preparation - Part 3: Sampling of static heaps Engrais et amendements minéraux basiques Échantillonnage et préparation de l'échantillon - Partie : Échantillonnage des tas statiques This European Standard was approved by CEN on 12 June 2016 Düngemittel und Kalkdünger - Probenahme und Probenvorbereitung - Teil 3: Probenahme aus statischen Haufwerken CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member This European Standard exists in three official versions (English, French, German) A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions 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, 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 © 2016 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members Ref No EN 1482-3:2016 E BS EN 1482-3:2016 EN 1482-3:2016 (E) Contents Page European foreword Introduction Scope Normative references Terms and definitions 4.1 4.2 4.3 4.3.1 4.3.2 4.4 4.5 4.5.1 4.5.2 4.5.3 4.5.4 4.6 4.6.1 4.6.2 4.6.3 Sampling plans and quantitative data General Characterization of the lot to be sampled Sampling plan General Elements of the sampling plan Determination of the volume/mass of the lot Determination of sampling units and sampling points Determination of the number and location of the sampling units Minimum total number of sampling units Determination of sampling units from which incremental samples shall be taken Determination of the minimum number of sampling points from which sub-samples are to be taken Quantitative data Determination of the minimum mass of increments Mass of increments Aggregate/reduced and final samples 5.1 5.2 5.3 5.4 Incremental sampling methods General Sampling apparatus Procedure 11 Aggregate and reduced samples 12 6.1 6.2 6.2.1 6.2.2 Final samples 12 Division into final samples 12 Practical arrangements for final (laboratory) samples 12 Final sample packaging materials 12 Dealing with final samples 12 Sampling report 12 Annex A (informative) Determination of mass/volume of a static heap 13 A.1 Volume of a conical heap without edgewise limitation 13 A.2 Volume of a storage box, partly filled (rectangular base, three flanks closed) 13 A.3 Determination of the mass 14 Annex B (informative) Alternative method according to GOST 15 Bibliography 16 BS EN 1482-3:2016 EN 1482-3:2016 (E) European foreword This document (EN 1482-3:2016) has been prepared by Technical Committee CEN/TC 260 “Fertilizers and liming materials”, the secretariat of which is held by DIN This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by February 2017, and conflicting national standards shall be withdrawn at the latest by February 2017 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 EN 1482 “Fertilizers and liming materials — Sampling and sample preparation” consists of three parts: — Part 1: Sampling; — Part 2: Sample preparation; — Part 3: Sampling of static heaps According to the CEN-CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard: 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, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom BS EN 1482-3:2016 EN 1482-3:2016 (E) Introduction 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 essential elements 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 nutrient content of such fertilizers To achieve this, representative sampling is essential for reliable analytical results Competent authorities have limited resources for conformity assessment and these are most efficiently deployed at the downstream end of the supply chain The purpose of Regulation (EC) No 2003/2003 [1] is to ensure that the fertilizer meets European requirements and complies with the declaration of the required characteristics applied to it when delivered to a purchaser EN 1482-1:2007 might not fully satisfy the needs of Member States when a large quantity of fertilizer is stored in a static heap that cannot be realistically put into motion An evaluation was requested to be carried out by CEN to see what, if any, static heaps of fertilizer could be representatively sampled at affordable costs see (see [3]) The fundamental principle of representative sampling is that every particle has an equal chance of being sampled This principle cannot easily be complied with in the case of bulk static heaps of solid fertilizers as a large proportion of the material cannot practically be reached by any sampling device Wherever possible, this fertilizer should be sampled during transfer, during the building up of the heap, during dispatch or where it can practically be moved solely for sampling purposes However, in some cases, sampling in the way described is not practicable The European Commission asked CEN/TC 260/WG to draft a European Standard in response to mandate M/454, which requires the development of a method of sampling static heaps that could not be sampled according to EN 1482-1:2007 This states that the sampling of static heaps should only be carried out when the product is in motion In response to the mandate, sampling methods to sample static heaps have been developed and standardized as specified in this document BS EN 1482-3:2016 EN 1482-3:2016 (E) Scope This European Standard is applicable to the sampling of mineral fertilizers and liming materials supplied or ready for supply to third parties, as a lot or in smaller lots, where such supply or readiness for supply is subject to legal requirements This European Standard specifies plans and methods of sampling of a lot of solid fertilizer or liming material, if sampling in motion is not possible, to obtain samples from static bulk heaps in order to ascertain compliance with legal requirements, in particular in relation to the accuracy of compulsory or permitted statutory declarations The methods specified in this document are not applicable to obtain samples for physical analysis or for the chemical analysis which may be altered by particle granulometric segregation This European Standard is applicable to single nutrient fertilizers, to uniform complex fertilizers and to milled or granulated liming materials The methods described in this document are not suitable for sampling other types of fertilizer, for example blended fertilizers NOTE The term 'fertilizer' is used throughout the body of this European Standard and includes liming materials unless otherwise indicated 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 Terms and definitions For the purposes of this document, the terms and definitions given in EN 1482-1:2007 and the following apply 3.1 fertilizer solid inorganic material designated for use as a fertilizer including liming materials 3.2 sampling point point in the sampling unit from which a sub-sample is taken Note to entry: For the definition of sub-sample, see EN 1482–1:2007, Note in 3.5 3.3 static heap quantity of fertilizer stored in bulk in a single mass Sampling plans and quantitative data 4.1 General The objective of sampling is to acquire a sample of the lot to establish its composition and properties The methods to be used for sampling static heaps are specified in the following clauses BS EN 1482-3:2016 EN 1482-3:2016 (E) 4.2 Characterization of the lot to be sampled Before a sampling plan is determined, a description of the characteristics of the lot that is intended to be sampled shall be undertaken In particular, the following physical characteristics shall be noted: — kind/type, — texture, — colour, — storage conditions, e.g uncovered/covered, — foreign matters If the owner of the material is applying the same description and statutory information to the whole lot, sampling should proceed in accordance with this document Only if there is evidence of deterioration or contamination should consideration be given to the dividing of the lot into parts from which separate samples should be taken 4.3 Sampling plan 4.3.1 General The sampling plan shall be determined after the characteristics according to 4.2 have been considered Any variations from the stated sampling plan shall be documented in written form The sampling plan shall define the course of the sampling process, and associated provisions, in reproducible manner Sampling only around the base of the heap or from a single part of the heap does not supply a representative sample 4.3.2 Elements of the sampling plan Within the sampling plan, the following elements shall be stated: — boundary of the lot, — determination of the volume/mass of the lot, — determination of the number and location of sampling units, — determination of sampling units from which the increments shall be taken, — if necessary, preparation of a sketch-map of the sampling areas (see Figure 1), — determination of the minimum number of sampling points from which sub-samples are to be taken to form the incremental sample, — determination of minimum volume/mass of increments BS EN 1482-3:2016 EN 1482-3:2016 (E) Key 1 to 32 + top ring second ring third ring fourth ring conveyor belt number of sampling units of equivalent surface 10 random selected sampling units for sampling sampling points (random distribution in the sampling unit) sampling units (180° each) sampling units (60° each) sampling units (45° each) 16 sampling units (22,5° each) Characteristics of the heap: angle of repose: 36 ° base diameter: 12 m circumference: 37,70 m height: ridge: volume: 5,3 m 8m 200 m3 Figure — Example of sampling plan for a conical heap (developed) BS EN 1482-3:2016 EN 1482-3:2016 (E) 4.4 Determination of the volume/mass of the lot The volume/mass of the lot should either be determined by reference to production/purchase/sales records of the owner or, if this is not possible, shall be estimated by the methods described in Annex A 4.5 Determination of sampling units and sampling points 4.5.1 Determination of the number and location of the sampling units The total minimum number of sampling units depends on the size of the lot Each sampling unit will be represented by approximately the same surface area 4.5.2 Minimum total number of sampling units The total number of sampling units into which the lot has to be divided shall be determined in accordance with Table Table — Number of sampling units that the lot needs be divided into 25 or less Lot size t More than 25 and up to 400 More than 400 Minimum number of sampling units 10 The nearest whole even number above the square root of times the quantity, in tonnes, present 40 4.5.3 Determination of sampling units from which incremental samples shall be taken Select randomly a minimum of 10 sampling units from the total number of sampling units determined in accordance with 4.5.2 using random number tables or a random number generator Incremental samples shall be taken from the selected sampling units 4.5.4 Determination of the minimum number of sampling points from which sub-samples are to be taken The number of sub-samples to be taken from the material in the selected sampling units shall be determined by reference to the minimum quantity of the incremental sample required according to 4.6.2 and the quantity of material delivered on each occasion by the sampling device Sub-samples shall comprise of a quantity of material taken at randomly selected points in each selected sampling unit These shall be mixed to form the incremental sample from that unit EXAMPLE Minimum quantity of incremental sample 250 g Sampling device delivers approximately 100 g from each point Sub-samples to be taken from three randomly selected points in the unit 4.6 Quantitative data 4.6.1 Determination of the minimum mass of increments One incremental sample shall be taken from each selected sampling unit All increments shall have approximately the same mass The required size of each incremental sample shall be considered when choosing the sampling device and the sampling method BS EN 1482-3:2016 EN 1482-3:2016 (E) 4.6.2 Mass of increments The incremental sample from any one sampling unit should be at least 250 g For liming materials coarser than 80 % passing 0,315 mm the mass of each increment should be at least 500 g 4.6.3 Aggregate/reduced and final samples Incremental samples from the static heap should be dealt with in accordance with EN 1482-1:2007, 4.3.2 to 4.3.4 Incremental sampling methods 5.1 General All sampling operations should be carried out in such a way as to minimize changes to sample properties, e.g moisture content In every case, the objective shall be to gain a sample that is representative of the lot with regard to the chemical composition An assessment should be carried out to determine any safety measures that should be taken 5.2 Sampling apparatus The sampling apparatus shall be clean, dry and inert (i.e fabricated of materials that will not affect the characteristics of the fertilizers to be sampled) The sampling apparatus shall be suitable to remove the required volume/mass The design of the apparatus for sampling should ensure that — a complete discharge is possible; — no contamination of the test material occurs; — the width of the opening should not be less than three times the size of the largest particle of the fertilizer Increments from static heaps can be taken by the following sampling apparatus: — sampling spear (with or without compartments) (see Figure 2); — for wet liming materials a tube shovel can be used (see Figure 3), or other suitable device BS EN 1482-3:2016 EN 1482-3:2016 (E) Figure — Sampling spears 10 BS EN 1482-3:2016 EN 1482-3:2016 (E) Dimensions in mm Figure — Sampling tube shovel for wet liming materials 5.3 Procedure When sampling loose bulk heaps, it is important to get increments not only from the surface layer The uppermost layer of the heap shall be excluded from sampling if encrustations or other changes are visible that clearly deviate from the whole of the heap Exclusion of such parts of the test material from sampling shall be documented If increments are taken using a sampling spear, insert the spear into the surface at an angle of 45° to the base of the static heap or at right angles to the surface layer (see Figure 4) 11 BS EN 1482-3:2016 EN 1482-3:2016 (E) If increments are taken from wet liming materials using a tube shovel, insert the tube shovel into the surface at an angle of 45 ° to the base of the static heap or at right angles to the surface layer (see Figure 4) Figure — Sampling of a conical heap using a spear The dotted line represents the depth the sampling device can practically reach 5.4 Aggregate and reduced samples All incremental samples shall be mixed together to form an aggregate sample which shall be dealt with in accordance with EN 1482-1:2007, Clause 6 Final samples 6.1 Division into final samples Final samples shall be obtained by division of the aggregate sample in accordance with EN 1482-1:2007, Clause 6.2 Practical arrangements for final (laboratory) samples 6.2.1 Final sample packaging materials The practical arrangements for final (laboratory) samples shall be in line with the requirements as specified in EN 1482-1:2007, Clause 6.2.2 Dealing with final samples Final samples in containers shall be dealt with in accordance with EN 1482-1:2007, 8.2, 8.3, 8.4, and 8.5 Sampling report The sampling report shall comply with EN 1482-1:2007, Clause as appropriate for bulk static heaps NOTE 12 It can be advantageous to photograph the heap and include this with the report BS EN 1482-3:2016 EN 1482-3:2016 (E) Annex A (informative) Determination of mass/volume of a static heap A.1 Volume of a conical heap without edgewise limitation An example is given in Figure A.1 Calculate the volume of the lot to be sampled, V, according to Formula (A.1) V= where d h d ×π × h 12 (A.1) is the diameter of the base of the cone; is the height of filling Figure A.1 — Conical heap A.2 Volume of a storage box, partly filled (rectangular base, three flanks closed) An example is given in Figure A.2 Calculate the volume of the lot to be sampled, V, according to Formula (A.2) V= × b × (l × h + l × a + d × a ) (A.2) 13 BS EN 1482-3:2016 EN 1482-3:2016 (E) where l b a h d is the distance between the base of the angle of repose and the back wall; is the width of the rectangular base; is the height of filling at the back wall; is the height of the apex; is the distance between apex and back wall Figure A.2 — Box shaped container A.3 Determination of the mass In the second step, estimate the mass using the density provided by the manufacturer 14 BS EN 1482-3:2016 EN 1482-3:2016 (E) Annex B (informative) Alternative method according to GOST In the experimental trial III, the method standardized in GOST 21560.0 (see [2]) was tested in parallel for the sampling of liming materials The principle is climbing the edge of the heap and sampling at regular intervals along a virtual edge of the heap Despite that this method is certainly an easier way to sample static heaps compared to full random sampling, this method is not suitable to ascertain compliance with legal requirements in the frame of the scope of EN 1482-3 However, GOST 21560.0 can be used as a screening test 15 BS EN 1482-3:2016 EN 1482-3:2016 (E) Bibliography [1] [2] [3] [4] 16 Regulation (EC) No 2003/2003 of the European Parliament and of the Council of 13 October 2003 relating to fertilisers, Official Journal L 304, 21/11/2003, P 0001 – 0194 GOST 21560.0, Mineral fertilizers — Methods of sampling and preparation of samples FprCEN/TR 17040, Sampling of fertilizers and liming materials - Report on experimental work of static heap sampling procedures EN 1482-2, Fertilizers and liming materials - Sampling and sample preparation - Part 2: Sample preparation This page deliberately left blank NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW British Standards Institution (BSI) BSI is the national body responsible for preparing British Standards and other standards-related publications, information and services BSI is incorporated by Royal Charter British Standards and other standardization products are published by BSI Standards Limited About us Reproducing extracts We bring together business, industry, government, consumers, innovators and others to shape their combined experience and expertise into standards -based solutions For permission to reproduce content from BSI publications contact the BSI Copyright & 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