SIST EN 15443:2011

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Trdna alternativna goriva - Metode za pripravo laboratorijskega vzorcaFeste Sekundärbrennstoffe - Verfahren zur Herstellung von LaboratoriumsprobenCombustibles solides de récupération - Méthodes de préparation des échantillons de laboratoireSolid recovered fuels - Methods for the preparation of the laboratory sample75.160.10Trda gorivaSolid fuelsICS:Ta slovenski standard je istoveten z:EN 15443:2011SIST EN 15443:2011en,de01-maj-2011SIST EN 15443:2011SLOVENSKI
STANDARDSIST-TS CEN/TS 15443:20071DGRPHãþD



SIST EN 15443:2011



EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 15443
March 2011 ICS 75.160.10 Supersedes CEN/TS 15443:2006English Version
Solid recovered fuels - Methods for the preparation of the laboratory sample
Combustibles solides de récupération - Méthodes de préparation des échantillons de laboratoire
Feste Sekundärbrennstoffe - Verfahren zur Herstellung von Laboratoriumsproben This European Standard was approved by CEN on 22 January 2011.
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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2011 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15443:2011: ESIST EN 15443:2011



EN 15443:2011 (E) 2 Contents Page Foreword .41 Scope .72 Normative references .73 Terms and definitions .74 Symbols and abbreviations .85 Principles of correct sample preparation .96 Apparatus . 116.1 Apparatus for sample division . 116.1.1 Riffle boxes . 116.1.2 Rotary sample dividers . 116.1.3 Shovels and scoops . 126.2 Apparatus for particle size reduction . 136.2.1 Coarse cutting mill or wood crusher . 136.2.2 Cutting mill . 136.2.3 Shredder . 136.3 Sieves . 146.4 Balance . 147 Sample preparation procedure . 147.1 General structure . 147.2 Step 1: Collection of the relevant information of the material to be sampled . 147.3 Step 2: Making a sample preparation plan . 157.3.1 General . 157.3.2 Retaining the minimum (sub-)sample size . 177.4 Step 3: Performing the sample preparation plan . 178 Methods for sample division . 189 Methods for reducing laboratory samples to sub-samples and general analysis samples . 209.1 General . 209.2 Initial sample division . 219.3 Initial mass determination . 219.4 Pre-drying . 219.5 Coarse cutting (particle size reduction to < 30 mm) . 229.6 Sample division of <30 mm material . 229.7 Particle size reduction of < 30 mm material to < 1 mm . 229.8 Sample division of < 1 mm material . 239.9 Particle size reduction of < 1 mm material to < 0,25 mm . 2410 Storage and labelling of sub-samples . 2411 Test report . 2412 Precision . 24Annex A (normative)
Determination of the changing shape factor . 26A.1 Introduction . 26A.2 Procedure . 26Annex B (normative)
Determination of the shape factor . 28B.1 Introduction . 28B.2 Procedure . 28Annex C (informative)
Examples of sample preparation. 29C.1 Introduction . 29SIST EN 15443:2011



EN 15443:2011 (E) 3 C.2 Example 1 pellets . 29C.3 Example 2 fluff . 29C.4 Large pieces SRF – Size-reduction and sub-population separation of field samples . 32Annex D (informative)
Data on the precision of sample preparation . 34D.1 Introduction . 34D.2 Scope . 34D.3 Trueness . 34D.4 Repeatability and reproducibility . 34D.5 Robustness . 35D.5.1 General . 35D.5.2 Type of solid recovered fuel . 35D.5.3 Level of particle size reduction . 35Bibliography . 37 SIST EN 15443:2011



EN 15443:2011 (E) 4 Foreword This document (EN 15443:2011) has been prepared by Technical Committee CEN/TC 343 “Solid recovered fuels”, the secretariat of which is held by SFS. 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 September 2011, and conflicting national standards shall be withdrawn at the latest by September 2011. This document supersedes CEN/TS 15443:2006. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN [and/or CENELEC] 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. This European Standard is one of series of European Standards dealing with sampling solid recovered fuel. EN 15442, Solid recovered fuels — Methods for sampling. EN 15443, Solid recovered fuels — Methods for the preparation of the laboratory sample. This document differs from CEN/TS 15443:2006 mainly as follows: a) results of interlaboratory tests supplemented as an informative Annex D; b) whole document editorially revised. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: 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, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
SIST EN 15443:2011



EN 15443:2011 (E) 5 Introduction Solid recovered fuels (SRF's) are a major source of renewable energy. European Standards are needed for production, trade and use of solid recovered fuels. For sampling and sample preparation of solid recovered fuels the following European Standards can be used: EN 15442, Solid recovered fuels — Methods for sampling; EN 15443, Solid recovered fuels — Methods for the preparation of the laboratory sample. These European Standards can be used by production and trading of solid recovered fuels. They are also useful for buyers of solid recovered fuels, regulators, controllers and laboratories. Figure 1 shows the links between the essential elements of a testing program. The sample preparation technique adopted depends on a combination of different characteristics of the material and circumstances encountered at the sampling location. The determining factors are:  the type of solid recovered fuel;  the physical behaviour of the specific solid recovered fuel;  the (expected) degree of heterogeneity (e.g. monostreams, mixed fuels, blended fuels). For the sample preparation of solid biofuels prEN 14780 is available [1]. For the characterization of waste
EN 15002 is available [2]. SIST EN 15443:2011



EN 15443:2011 (E) 6
Figure 1 — Links between the essential elements of a testing program
SIST EN 15443:2011



EN 15443:2011 (E) 7 1 Scope This European Standard specifies methods for reducing combined samples to laboratory samples and laboratory samples to sub-samples and general analysis samples. The methods described in this European Standard may be used for sample preparation, for example, when the samples are to be tested for bulk density, biomass determination, durability, particle size distribution, moisture content, ash content, ash melting behaviour, calorific value, chemical composition, and impurities. The methods are not intended to be applied to the very large samples required for the testing of bridging properties. 2 Normative references The following referenced documents are indispensable for the application 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. EN 15297, Solid biofuels — Determination of minor elements — As, Cd, Co, Cr, Cu, Hg, Mn, Mo, Ni, Pb, Sb, V and Zn EN 15357:2011, Solid recovered fuels — Terminology, definitions and descriptions CEN/TS 15414-1:2010, Solid recovered fuels —Determination of moisture content using the oven dry method — Part 1: Determination of total moisture by a reference method CEN/TS 15414-2:2010, Solid recovered fuels — Determination of moisture content using the oven dry method — Part 2: Determination of total moisture by a simplified method EN 15414-3, Solid recovered fuels — Determination of moisture content using the oven dry method — Part 3: Moisture in general analysis sample EN 15415-11), Solid recovered fuels — Determination of particle size and particle size distribution — Part 1: Screen method for small dimension particles EN 15442, Solid recovered fuels — Methods for sampling 3 Terms and definitions For the purposes of this document, the terms and definitions given in EN 15357:2011 and the following apply. 3.1 combined sample sample consisting of all the increments taken from a lot or a sub-lot NOTE The increments can be reduced by division before being added to the combined sample. 3.2 general analysis sample sub-sample of a laboratory sample having a nominal top size of 1 mm or less and used for a number of chemical and physical analyses 3.3 increment portion of solid recovered fuel extracted in a single operation of the sampling device
1) To be published. SIST EN 15443:2011



EN 15443:2011 (E) 8 3.4 laboratory sample sample sent to or received by the laboratory NOTE 1
When the laboratory sample is further prepared (reduced) by subdividing, mixing, grinding, or by combinations of these operations, the result is the test sample. When no preparation of the laboratory sample is required, the laboratory sample is the test sample. A test portion is removed from the test sample for the performance of the test or for analysis. NOTE 2
The laboratory sample is the final sample from the point of view of sample collection but it is the initial sample from the point of view of the laboratory. NOTE 3
Several laboratory samples may be prepared and sent to different laboratories or to the same laboratory for different purposes. When sent to the same laboratory, the set is generally considered as a single laboratory sample and is documented as a single sample. 3.5 lot defined quantity of fuel for which the quality is to be determined 3.6 moisture analysis sample sample taken specifically for the purpose of determining total moisture 3.7 nominal top size d95 aperture size of the sieve used in EN 15415-1 through which at least 95 % by mass of the material passes 3.8 particle size reduction reduction of the nominal top size of a sample or sub-sample 3.9 sample quantity of fuel, representative of a larger mass for which the quality is to be determined 3.10 sample division reduction of the mass of a sample or sub-sample 3.11 sub-sample portion of a sample 3.12 test portion sub-sample of a laboratory sample consisting of the quantity of material required for a single execution of a test method 4 Symbols and abbreviations For the purposes of this document, the following symbols and abbreviated terms apply. α is a constant in third power law d95 is the nominal top size in mm m is the mass of a sample in gram SIST EN 15443:2011



EN 15443:2011 (E) 9 M is moisture in percent by weight f
is the shape factor 5 Principles of correct sample preparation The main purpose of sample preparation is that a sample is reduced to one or more test portions that are in general smaller than the original sample. The main principle for sample preparation is that the composition of the sample as taken on site shall not be changed during each step of the sample preparation and that possible requirements of the analysis methods to be performed are obeyed. Each sub-sample shall be representative for the original sample. To reach this goal every particle in the sample before sample preparation shall have an equal probability of being included in the sub-sample retained after sample preparation. Also the loss of moisture and other volatile components shall be minimised if these components are analysed or influence the properties to be analysed. Two basic methods are used during the sample preparation. These methods are:  sample division;  particle size reduction of the sample. For granular materials generally the principle of the third-power law is accepted and shall be respected at each sample division step. The equation for this third power law is shown in Equation (1): 395
d.m×> (1) where m
is the mass retained after each sample division step in g; d95 is the nominal top size in mm; α is a constant over the whole sample preparation procedure for a particular material in g/mm3. The value and unit of constant α is fixed by the nominal particle size, d95, and the sample size, m, of the sample before sample preparation. EXAMPLE A sample of 10 kg of SRF fluff has d95 of 50 mm. For the analysis is a test portion of 5 g required. The third power law results in α = 10 000 g divided by 50 mm to the third power. The value of α is now 0,08 g/mm3. Using this value in Equation (1) for a reduced sample size results in a nominal top size for the particles in the test portion of 3,97 mm (cube root of 5,0 g divided by 0,08 g/mm3). Below in the table are shown the figures. m in g αααα In g/mm3
d95 in mm 10 000 0,08 50 5 0,08 3,97
Table 1 shows the resulting reduction factors for the minimum (sub-)sample size, if a certain reduction of the nominal top size is chosen and the third-power law is respected. The reduction factor of the nominal top size can be calculated by dividing the current nominal top size by the proposed nominal top size after size reduction. SIST EN 15443:2011



EN 15443:2011 (E) 10 Table 2 shows the resulting reduction factors for the minimum nominal top size, if a certain reduction of the (sub-)sample size is chosen and the third-power law is respected. The reduction factor of the minimum
(sub-)sample size can be calculated by dividing the current minimum (sub-)sample size by the proposed minimum (sub-)sample top size after size reduction. Equation (1) can be used to calculate the exact values for each specific situation. Table 1 — Common values for desired reduction factor minimum
(sub-)sample size
Table 2 — Common values for desired reduction factor nominal top size
Chosen reduction factor of the nominal top size Resulting reduction factor for the minimum (sub-)sample size
Desired reduction factor for the minimum
(sub-)sample size Necessary reduction factor of the nominal top size 1,5 3,4
2 1,3 2 8
3 1,4 3 27
4 1,6 4 64
5 1,7 5 125
10 2,2 6 216
20 2,7 7 343
50 3,7 8 512
80 4,3 9 729
100 4,6 10 1 000
200 5,8 20 8 000
500 7,9 30 27 000
1 000 10,0
For SRF, however, many materials turn out to be far from granular. For example in fluff the particles turn out to be predominantly flat. Therefore, for solid recovered fuels, a correction can made for non-granular materials. Care is needed to avoid loss of fine particles and volatile components such as moisture and mercury during milling and other operations. If a sub-sample is required for the determination of moisture content, then the sample preparation shall be carried out by a procedure that does not conflict with the requirements of CEN/TS 15414-1, CEN/TS 15414-2 or EN 15414-3. It is recommended that, if moisture content of the material (as sampled) is to be determined, a separate moisture analysis sample is taken (as there is a risk of reducing the moisture content by sample preparation operations). If a sub-sample is required for the determination of mercury content, then the sample preparation shall be carried out by a procedure that does not conflict with the requirements of EN 15297. It is recommended that, if mercury content of the material (as sampled) is to be determined, a separate mercury analysis sample is taken (as there is a risk of reducing the mercury content by sample preparation operations). For materials that have to be examined for moisture and mercury content, care shall be taken for any significant heat build-up and risk of loss of moisture and mercury. SIST EN 15443:2011



EN 15443:2011 (E) 11 6 Apparatus 6.1 Apparatus for sample division 6.1.1 Riffle boxes A riffle box shall have at least 16 slots and an even number of slots, with adjacent slots directing material into different sub-samples, and the width of the slots shall be at least 3 times the nominal top size of the material to be riffled (see Figure 2).
Key 1 slot, width is at least 3 times the nominal top size of the material Figure 2 — Example of a riffle box 6.1.2 Rotary sample dividers A rotary sample divider shall have a feeder device adjusted so that the divider rotates at least 20 times while the sample is being divided. See Figure 3 for an example of a rotating divider. The manufacturer’s instruction manual shall always be followed. The inner dimensions of the equipment where the sample is feed shall be at least 3 times as wide as the nominal top size of the material to be processed. SIST EN 15443:2011



EN 15443:2011 (E) 12
Key 1 feeder 2 funnel 3 rotating receiver 4 divided sample Figure 3 — Example of a rotary sample divider 6.1.3 Shovels and scoops A shovel or scoop used for manual sample division shall have a flat bottom, edges raised high enough to prevent particles rolling off, and shall be at least 3 times as wide as the nominal top size of the material to be processed. See Figures 4 and 5 for examples of a scoop and a shovel respectively.
Key d is the nominal top size Figure 4 — Example of a scoop SIST EN 15443:2011



EN 15443:2011 (E) 13
Key l
is the length of the shovel A - A sectional view Figure 5 — Example of a shovel 6.2 Apparatus for particle size reduction 6.2.1 Coarse cutting mill or wood crusher Coarse cutting mills are used for cutting materials into lengths of about 10 mm to 30 mm (depending on the solid recovered fuel and the analyses to be performed). The equipment shall have a minimum of drying effect either by heating the materials or blowing air through them. The equipment shall be designed so that it does not lose dust or contaminate the material with pieces of metal, and shall be easy to clean. A cutting mill with no screens may be suitable for small quantities. 6.2.2 Cutting mill Cutting mills are used for particle size reduction of materials used as solid recovered fuels from about 10 mm to 30 mm down to about 1 mm or less (depending on the solid recovered fuel and the analyses to be performed). The mill shall be provided with screens of various aperture sizes covering this range, including an appropriate sieve to control the nominal top size of the material produced. Other apparatus may be used provided that they are designed so that they do not get blocked with the material that is being processed. Avoid the use of cutting mills whose cutting faces contain significant quantities of an element that is to be determined in the analysis. NOTE Cross beater mills can be used without any excessive dusting, when fitted with dust filters (like a filter sock) between the mill and the receiving container. They are suitable for final grinding of hard, wood type materials after the
pre-grinding with cutting type mills. 6.2.3 Shredder A shredder is an apparatus with a rotor equipped with hammers that shred the material which is fed to the shredder. Shredders are used for reducing the particle size down to 30 mm. In case of hardy and strong materials it can be necessary to perform the particle size reduction in more than one step. The use of SIST EN 15443:2011



EN 15443:2011 (E) 14 shredders for particle size reduction causes a risk of losing moisture and fine fractions. Therefore the use of shredders shall be avoided when possible. Unfortunately many types of solid recovered fuel contain plastics and metals and make therefore the use of a shredder necessary. 6.3 Sieves A wire-mesh sieve with an aperture size of 1,00 mm is required to check the nominal top size of general analysis samples. A wire-mesh sieve with an aperture size of 0,250 mm will be required if sub-samples with this as the nominal top size are required. 6.4 Balance A balance is required that is capable of determining the mass of samples to an accuracy of 0,1 % of the sample mass, and the mass of sub-samples to an accuracy of 0,1 % of the sub-sample mass. 7 Sample preparation procedure 7.1 General structure Figure 6 outlines the general procedure that shall be followed in order to perform the sample preparation according to this European Standard.
Figure 6 — General sample preparation procedure 7.2 Step 1: Collection of the relevant information of the material to be sampled In the first step of sample preparation information shall be collected about the material to be sampled: a) the minimum sample size out of the sampling plan; b) the actual size of the sample, m0; c) the nominal top size of the sample; d) the shape factor of the sample; SIST EN 15443:2011



EN 15443:2011 (E) 15 e) the requirements in terms of size reduction for the analysis that need to be performed; f) the required amounts for each of the size fractions and their restrictions to the sample preparation methods. Sample preparation prepares a sample for a number of tests which will be performed on the sample. Some of these tests require no particle size reduction or drying of the material in the sample. Other tests require very tiny homogenized sub-samples with small particle sizes. A sample preparation plan shall have to meet all these requirements. 7.3 Step 2: Making a sample preparation plan 7.3.1 General This subclause specifies the making of a sample preparation plan. The actual making of the sample preparation plan is the most crucial phase during sample preparation. Sample preparation is a combination of sample division and particle size reduction. Until what level a sample of solid recovered fuel shall be prepared on site depends on available equipment on site, the requirements of the laboratory and the preferences of the client of the sampling activities. These two essential activities are specified below. Sample division The aim of sample division of a sub-sample is to reduce the mass remaining sub-sample or to make several duplicate sub-samples out of one original sub-sample available. During the performance of sample division it is of eminent importance that the minimum sub-sample size shall be retained in order to sustain the representatively of the sub-sample for the original combined sample. Clause 7 describes the available methods for sample division. Particle size reduction of a sample The aim of particle-size reduction is to reduce the nominal top size of the particles in order to reduce the minimum
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