INTERNATIONAL ISO

STANDARD 14780

First edition
2017-04

Solid biofuels — Sample preparation

Biocombustibles solides — Préparation des échantillons

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Reference number
ISO 14780:2017(E)

© ISO 2017
ISO 14780:2017(E)


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COPYRIGHT PROTECTED DOCUMENT

© ISO 2017, Published in Switzerland
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
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Contents Page

Foreword......................................................................................................................................................................................................................................... iv
Introduction...................................................................................................................................................................................................................................v
1 Scope.................................................................................................................................................................................................................................. 1
2 Normative references....................................................................................................................................................................................... 1
3 Terms and definitions...................................................................................................................................................................................... 1
4 Symbols........................................................................................................................................................................................................................... 2
5 Principles of correct sample reduction......................................................................................................................................... 2
6 Apparatus...................................................................................................................................................................................................................... 2
6.1 Apparatus for sample division................................................................................................................................................... 2
6.1.1 General...................................................................................................................................................................................... 2
6.1.2 Riffle boxes............................................................................................................................................................................. 2
6.1.3 Rotary sample dividers............................................................................................................................................... 3
6.1.4 Shovels and scoops......................................................................................................................................................... 4

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6.2 Apparatus for particle size-reduction.................................................................................................................................. 5
6.2.1 Coarse cutting mill or wood crusher............................................................................................................... 5
6.2.2 Cutting mill............................................................................................................................................................................ 5
6.2.3 Axe................................................................................................................................................................................................. 6
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6.2.4 Hand saw................................................................................................................................................................................. 6
6.2.5 Sieves.......................................................................................................................................................................................... 6
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6.2.6 Balance...................................................................................................................................................................................... 6
7 Sample reduction — General principles....................................................................................................................................... 6
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8 Methods for sample division..................................................................................................................................................................... 8

8.1 General............................................................................................................................................................................................................ 8
8.2 Riffling............................................................................................................................................................................................................. 9
8.3 Strip mixing................................................................................................................................................................................................ 9
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8.4 Long pile-alternate shovel method......................................................................................................................................... 9

8.5 Rotary divider........................................................................................................................................................................................ 10
8.6 Coning and quartering.................................................................................................................................................................... 10
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8.7 Mass reducing straw-like material (handful sampling).................................................................................... 10

9 Method for reducing laboratory samples to sub-samples and general analysis samples.....11
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9.1 Mixing........................................................................................................................................................................................................... 11
9.2 Initial sample division.................................................................................................................................................................... 11
9.3 Pre-drying................................................................................................................................................................................................. 11
9.4 Coarse cutting (particle size reduction to <31,5 mm)........................................................................................ 12
9.5 Sample division of <31,5 mm material............................................................................................................................. 12
9.6 Particle size reduction of <31,5 mm material to <1 mm................................................................................... 12
9.7 Sample division of <1 mm material.................................................................................................................................... 13
9.8 Particle size reduction of <1 mm material to <0,25 mm................................................................................... 13
10 Storage and labelling.....................................................................................................................................................................................13
11 Performance characteristics..................................................................................................................................................................13
Annex A (informative) Precision in relation to division method..........................................................................................14
Annex B (informative) Scheme of sample preparation for samples from single delivery..........................19
Annex C (informative) Scheme of sample preparation for samples from continuous delivery............20
Bibliography.............................................................................................................................................................................................................................. 22

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Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www​.iso​.org/​directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www​.iso​.org/​patents).

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Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
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For an explanation on the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO’s adherence to the
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World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following
URL: www​.iso​.org/​iso/​foreword​.html.
This document was prepared by Technical Committee ISO/TC 238, Solid biofuels.
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Introduction
Biofuels are a major source of renewable energy. International standards are needed for production,
trade and use of solid biofuels. For sampling of solid biofuels, see ISO 18135.
This document can be used in regard to production, controlling and analysis of solid biofuels in general.
This document was developed with significant content from EN 14780:2011.

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INTERNATIONAL STANDARD ISO 14780:2017(E)

Solid biofuels — Sample preparation

1 Scope
This document defines methods for reducing combined samples (or increments) to laboratory samples
and laboratory samples to sub-samples and general analysis samples and is applicable to solid biofuels.
The methods defined in this document can be used for sample preparation, for example, when the
samples are to be tested for calorific value, moisture content, ash content, bulk density, durability,
particle size distribution, ash melting behaviour, chemical composition, and impurities.

2 Normative references
The following documents are referred to in the text in such a way that some or all of their content

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constitutes requirements 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.
ISO 3310-1, Test sieves — Technical requirements and testing — Part 1: Test sieves of metal wire cloth
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ISO 16559, Solid biofuels — Terminology, definitions and descriptions
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ISO 18134-1, Solid biofuels — Determination of moisture content — Oven dry method — Part 1: Total
moisture — Reference method
ISO 18134-2, Solid biofuels — Determination of moisture content — Oven dry method — Part 2: Total
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moisture — Simplified procedure

ISO 18135, Solid Biofuels — Sampling
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3 Terms and definitions

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For the purposes of this document, the terms and definitions given in ISO 16559 and the following apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
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— IEC Electropedia: available at http://​w ww​.electropedia​.org/​

— ISO Online browsing platform: available at http://​w ww​.iso​.org/​obp
3.1
nominal top size
aperture size of the sieve through which at least 95 % by mass of the material passes
Note 1 to entry: For pellets (and other long materials), the diameter is used to determine the nominal top size.

Note 2 to entry: Includes additional information not found in ISO 16559.

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4 Symbols

Mp moisture loss, in percentage

msample,1 initial mass of the sample, g

msample,2 mass of the sample after pre-drying, g

W width and is at least 2,5 times the nominal top size of the material and should be wide
enough for normal oversized material particles to enter the sampling device

5 Principles of correct sample reduction

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 reduction is that
the composition of the sample as taken on site shall not be changed during each stage of the sample
preparation. Each sub-sample shall be representative of the original sample. To reach this goal, every
particle in the sample before sample division shall have an equal probability of being included in the

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sub-sample following sample division. Two basic methods are used during the sample preparation.
These methods are:
— sample division;
— particle size-reduction of the sample. N
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CAUTION — Avoid loss of moisture and fine particles during milling and other operations.
Because of the risk of changes in the moisture content (loss of moisture), a sub-sample (moisture
analysis sample) shall be separated at the earliest possible stage of the sample preparation procedure.
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As an alternative, a separate moisture analysis sample may be taken. The sample reduction shall be
carried out by a procedure that does not conflict with the requirements of ISO 18134-1 or ISO 18134-2.
For materials that have to be examined for moisture content, care should be taken to avoid any
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significant heat build-up and risk of drying.

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6 Apparatus
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6.1 Apparatus for sample division

6.1.1 General

Sample division is the process of reducing the mass of the sample without reducing the size of the
particles. This subclause gives some suitable apparatus for this purpose. To determine the correct use
of each apparatus for different purposes, refer to Clause 8.
If the nominal top size of the sample is not known, a value of this parameter has to be assumed. After
the sample reduction, the assumed value should be compared to the actual value to assure that the
requirements of the apparatus for sample division and sample size used are met.

6.1.2 Riffle boxes

A riffle box should have an equal number of slots and at least six at each side (preferably more if
possible), with adjacent slots directing material into different sub-samples, and the width of the slots
shall be at least 2,5 times the nominal top size of the material to be riffled (see Figure 1).

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1 width

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Figure 1 — Example of a riffle box

6.1.3 Rotary sample dividers

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The inner dimensions of the equipment where the sample is fed shall be at least 2,5 times as wide as the
nominal top size of the material to be processed and should be large enough to handle normal oversized
material particles. The rotary sample divider shall have a feeder device adjusted, so that the number
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of compartments multiplied by the number of rotations shall not be less than 120 while the sample is
being divided. See Figure 2 for an example of a rotating divider.
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1 feeder
2 funnel
3 rotating receivers
4 divided sample

Figure 2 — Example of a rotary sample divider

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6.1.4 Shovels and scoops

A shovel or scoop are tools used for manual sample division. They shall have a flat bottom, with
edges raised high enough to prevent particles from rolling off, shall be at least 2,5 times as wide as
the nominal top size of the material to be processed, and should be large enough to handle normal
oversized material particles. See Figures 3 and 4 for examples of scoops and a shovel, respectively.

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1 width
2 height

Figure 3 — Example of scoops

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Figure 4 — Example of a shovel
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6.2 Apparatus for particle size-reduction
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CAUTION — When analysing metals (major or minor elements), take care that there is no
contamination from the sample preparation or reduction equipment.
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6.2.1 Coarse cutting mill or wood crusher

Coarse cutting mills can be used for cutting materials into lengths of about 10 mm to 30 mm (depending
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on the biofuel and the analyses to be performed). Drying of the material during coarse cutting shall be
avoided by limiting heat production and air flow through the material. The equipment shall be designed
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so that it does not lose dust or contaminate the material with pieces of metal, and shall be easy to clean.
NOTE To prevent moisture losses during particle size reduction, a cutting mill or crushing mill with as low a
cutting or crushing speed as possible is preferred.

6.2.2 Cutting mill

Cutting mills can be used for reducing the nominal top size of materials used as biofuels from
about 10  mm to 30  mm down to about 1  mm or less (depending on the biofuel 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.

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6.2.3 Axe

An axe is used for cutting wood logs or coarse material down to a maximum 30 mm thickness or suitable
size to be processed in a cutting mill provided with a 30 mm sieve.

6.2.4 Hand saw

A hand saw is used to saw off wood logs or coarse material down to a maximum 30 mm thickness or
suitable size to be processed in a cutting mill provided with a 30 mm sieve.
A chain saw may contaminate the sample by chain oil and should therefore not be used. A saw machine
should not be used for size reduction to avoid the risk of losing moisture in the sample as a result of heat
caused by friction.

6.2.5 Sieves

A wire-mesh sieve with an aperture size of 1 mm, in accordance with ISO 3310-1, is recommended to
check the nominal top size of general analysis samples. A wire-mesh sieve with an aperture size of
0,25 mm will be recommended if sub-samples with this nominal top size are required.

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6.2.6 Balance

A balance is required that is capable of determining the mass of samples to an accuracy of 0,1 % of the
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sample mass, and the mass of sub-samples to an accuracy of 0,1 % of the sub-sample mass.
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7 Sample reduction — General principles
For every sample division stage to be carried out, it is important that a sufficient mass of material
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is retained, otherwise the sub-samples produced or the test portions to be taken may not be
representative of the original sample. Due to various shape and size of different solid biofuels, different
methods for determination of minimum sample masses have to be applied. Table 2 gives a guideline for
minimum masses to be retained after each sample division stage, depending on the nominal top size of
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the material.
Regarding pellets, the pellets diameter shall be considered the nominal top size and the opening of the
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equipment shall be large enough for the longest pellets to pass through.
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In addition to the minimum masses stated in Table 2, the mass after sample division shall be sufficiently
large for the actual test or tests to be performed. Table 1 gives a guideline for the selection of the method
to be applied to determinate the minimum sample mass to be retained after each sample division stage.
Supplementary requirements concerning the masses of the test portions are given in international
standards for test methods of solid biofuels.

Table 1 — Guideline to choose a method to determine the minimum masses to be retained

during sample division stages
1 2 3 4
Material Bulk material of Large pieces Straw-like material Irregular/mixed
less than or equal >100 mm material, with a low bulk den- materials, e.g.
to 100 mm nominal e.g. wood logs or sity (≤BD 200 kg/ hogfuels, logging
top size as defined in briquettes m3) and lengths residues, bark
ISO 16559 >31,5 mm
Method for determi- Calculate the mini- Number of pieces Minimum sample To be determined ac-
nation of minimum mum sample mass should be stated, e.g. mass should be de- cording to fuel type
sample mass according to Table 2 10 pieces randomly fined, e.g. 500 g
collected

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Table 2 — Guideline for minimum masses to be retained during sample division stages,
applicable for material according to column 1 in Table 1
Nominal top size Minimum mass
mm g
100 15 000
63 4 000
45 1 500
31,5 500
16 350
8 250
3,15 100
1 30
0,25 10

According to particle size distribution, shape and density of particles, the calculation of minimum

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sample mass should be adapted to the methods given here at the best in practical terms.
Figure 5 summarizes the range of steps that can be taken during sample reduction.

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NOTE List of optional sub-sample extractions can not be exhaustive.

Figure 5 — Flow sheet for sample preparation and optional extraction of sub-samples

8 Methods for sample division

8.1 General
Combined samples may be divided into two or more laboratory samples and laboratory samples are
in general further divided in sub-samples (test portions). This clause describes the methods and
procedures for sample division. For every division step, the mass of retained material given in Table 2
shall be taken into account.

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8.2 Riffling
This may be used for materials that can be passed through the riffle without bridging. It is not suitable
for straw, bark, or other materials containing elongated particles, or for wet and/or sticky materials.
Brittle materials should be handled with care to avoid the production of fine materials. Place the whole
of the combined sample into one of the containers of the riffle so that it is evenly distributed throughout
the container. Place the other two containers in position under the riffle. Pour the contents of the
first container down the centre line of the riffle. Pour the biofuel sufficiently slowly to avoid bridging
occurring. Do not move the container from side to side (this would cause the end slots to receive less
biofuel). Discard the biofuel that falls into one of the containers, chosen at random. Repeat the riffling
process until a sub-sample of the required mass is obtained. See Figure 1 for an example of a riffle box.

8.3 Strip mixing

This may be used for all materials and will be a convenient method when a combined sample is to be
divided into a small number of laboratory samples. Place the whole combined sample on a clean, hard
surface and homogenize it by mixing with a shovel, and form into a strip at least 20 times as long as it is
wide. Distribute the sample along the length of the strip as evenly as possible, working randomly from
end to end. Building up the strip with several layers will increase the quality of the division.

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Obtain a laboratory sample by taking at least 20 increments from locations evenly spaced along the
length of the strip. Take each increment by inserting two plates vertically into the strip and removing
all the material from between the plates. The two plates should be inserted the same distance apart
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each time so that each increment contains the same quantity of material. The distance between the
plates should be at least 2,5 times the nominal top size and at least the length of normal oversized
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material particles. See Figure 6 for the principle of strip mixing.
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Figure 6 — Strip mixing

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1 increment
2 sampling frame
3 end plates

8.4 Long pile-alternate shovel method

This sub-sampling method is recommended for the reduction of samples in excess of approximately
50 kg. Place the entire combined sample on a clean and even floor and mix it thoroughly by manually
moving the material to form a long pile. Carry out this process at least three times to ensure thorough
mixing. When forming new piles, deposit each shovelful on the end of the new pile. Divide the last pile
into two equal piles by using a shovel. Place alternate shovel loads to either side and form into two piles
with at least 10 shovel loads (increments) in each pile. One pile is randomly selected and the process
is repeated, using appropriately smaller increments as the piles are getting smaller. For straw-like
material, this method may require excessive manual work.

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For samples in excess of 500 kg, a mechanical shovel should be considered and used if appropriate.

8.5 Rotary divider

A rotary sample divider is a mechanical method that can be used to reduce the mass of a sample. This
method is recommended for dry free flowing material. The rotary sample divider shall have a feeder
device adjusted, so that the number of compartments multiplied by the number of rotations shall not be
less than 120 while the sample is being divided. See Figure 2 for an example of a rotary divider.

8.6 Coning and quartering

This method may be used for materials such as sawdust and woodchips that can be manually worked
with a shovel. It is suitable for producing sub-samples of these materials down to approximately 1 kg.
Place the whole combined sample on a clean, hard surface. Shovel the sample into a conical pile, placing
each shovelful on top of the preceding one in such a way that the biofuel runs down all sides of the
cone and is evenly distributed and different particle sizes become well mixed. Repeat this process three
times, forming a new conical pile each time. Flatten the third cone by inserting the shovel repeatedly
and vertically into the peak of the cone to form a flat heap that has a uniform thickness and diameter
and is no higher than the blade of the shovel. Quarter the flat heap along two diagonals at right angles

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by inserting the shovel vertically into the heap (see Figure 7) (A sheet-metal cross may be used for this
operation if available). Discard one pair of opposite quarters. Repeat the coning and quartering process
until a sub-sample of the required size is obtained.
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For materials and particles that tend to roll off the pile and cause segregation, this method should only
be used when methods described in 8.2 to 8.5 cannot be applied.
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1 discard

Figure 7 — Coning and quartering

8.7 Mass reducing straw-like material (handful sampling)

This method is suitable for small sample sizes of straw-like material. Place the whole sample in an air-
tight bag and homogenize it by inverting and kneading the bag several times. Take several handfuls and
put them alternately into two piles. Homogenize the material remaining in the bag again, then remove
several more handfuls and add them alternately to the two piles. Continue like this until the material in
the bag is all used. At least 20 handfuls shall be placed into each of the two sub-samples.

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9 Method for reducing laboratory samples to sub-samples and general

analysis samples

9.1 Mixing
Mixing is recommended before each step of sample division. It should be noted that the sample division
does not ensure that samples are adequately mixed. Additional mixing can be achieved by pouring it
through a riffle (see 8.2) or a container-type divider (see Figure 2) three times, reuniting the parts after
each pass.
Beware that mixing may result in loss or gain of moisture.
If the material is too wet to handle, pre-drying should be carried out first.
NOTE 1 In theory, thorough mixing of a sample prior to its division reduces errors occurring in sample
preparation. In practice, this is not easy to achieve and some methods of hand mixing, e.g. forming and reforming
into a conical pile, can have the opposite effect, leading to increased segregation.

NOTE 2 If mechanical sample dividers are used in the course of preparation, an additional mixing step is
normally not necessary to meet the required precision.

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NOTE 3 Mechanical mixing can be useful at the final stage of preparation of test samples.

9.2 Initial sample division N

If the initial mass of the laboratory sample exceeds the minimum mass given in Table 2, the laboratory
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sample may be divided using one of the methods described in Clause 8.
If the material is too wet to handle, pre-drying should be carried out first.
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9.3 Pre-drying
Pre-drying of wet samples is in general carried out to minimize moisture loss in the subsequent sample-
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division processes, to facilitate the sample preparation processes, and to minimize biological activity.
If it is necessary to dry a sample by heating, it shall be dried in an oven at a temperature not exceeding
40 °C. All samples (including those that have been dried by heating) shall be spread out on a tray no
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more than a few particles deep and left for at least 24 h in the laboratory until they reach equilibrium
with the temperature and humidity in the laboratory.
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Before the laboratory sample or the divided laboratory sample according to 9.2 is subject to pre-drying,
determine the mass of the sample by weighing on a balance accurate to at least 0,1 % of the sample
mass. Record this mass as msample,1. After pre-drying and equilibrium with the surroundings, record
the mass as msample,2.
Calculate the moisture loss during pre-drying as a percentage of the initial mass of the sample as shown
in Formula (1):

msample,1 − msample,2
M p = 100 × (1)
msample,1
where

Mp is the moisture loss in percentage;

msample,1 is the initial mass of the sample in g;

msample,2 is the mass of the sample after pre-drying in g.

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Record the result to the nearest 0,1 %.

NOTE If the moisture content of the original sample is unimportant, e.g. only properties of the dry matter or
mechanical properties are to be determined or if a separate “moisture analysis sample” is separated or sampled
as well, the calculation of the moisture loss can be omitted. Also in this case, it is not necessary to obtain complete
equilibrium with the temperature and humidity in the laboratory.

For coarse materials, for example, 24 h under laboratory conditions is not enough to reach equilibrium
moisture content in all particles. Constancy in mass should be monitored by re-weighing at intervals at
e.g. 4 h. The sample material should be turned around from time to time during the equilibrium process.

9.4 Coarse cutting (particle size reduction to <31,5 mm)

If the material contains particles that will be retained on a 31,5 mm sieve:
— use a 31,5 mm sieve to separate the sample into a coarse fraction (retained on the 31,5 mm sieve)
and a fine fraction (passing the 31,5 mm sieve);
— process the coarse fraction using a coarse cutting mill so that it passes the 31,5 mm sieve;

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NOTE 1 Depending on the material, other mills than the cutting mill can be used.

— re-combine the processed coarse fraction and the fine fraction and homogenize the sample.

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If required, the above procedure may be used to achieve particle size reduction to a size below 31,5 mm
by the use of a suitable coarse cutting mill and sieve.
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NOTE 2 Grinding of the whole sample through the sieve fitted in the mill will produce the particle size needed.

9.5 Sample division of <31,5 mm material

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One of the methods described in Clause 8 shall be used for sample division.
Determine the masses of the containers into which the sub-samples are to be put before starting the
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division.
Weigh the sub-sample masses using a balance accurate to 0,1 %. The masses of retained sub-samples
shall comply with the values stated in Table 2.
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Seal the container immediately if a sub-sample is required for moisture content determination or
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another test for which it is important not to lose moisture.

When a sub-sample is to be used as a test portion, the sub-sample shall have a mass not less than the
minimum test-portion mass specified in the appropriate test method.

9.6 Particle size reduction of <31,5 mm material to <1 mm

Use a cutting mill for the preparation of the general analysis sample material <1 mm from the <31,5 mm
material. Carry out the process in several steps, if necessary, using a finer sieve in the mill at each step,
finishing with an appropriate sieve.
NOTE 1 Depending on the material, other mills than the cutting mill can be used.

NOTE 2 Grinding of the whole sample through the sieve fitted in the mill will produce the particle size needed
and it also homogenizes the sample at the same time.

EXAMPLE If the sample is to be reduced first to pass a 5 mm screen and then to pass a 1 mm screen:

— use a 5 mm sieve to separate the sample into a coarse fraction (retained on the 5 mm sieve) and a fine fraction
(passing the 5 mm sieve);

— process the coarse fraction using a cutting mill containing a 5 mm screen;

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— re-combine the processed coarse fraction and the fine fraction and homogenize;

— use a 1 mm sieve to separate the sample into a coarse fraction (retained on the 1 mm sieve) and a fine fraction
(passing the 1 mm sieve);

— process the coarse fraction using a cutting mill containing a 1 mm screen;

— re-combine the processed coarse fraction and the fine fraction and homogenize the sample.

If the material contains seeds or grains, there is a risk that they will rotate in the mill or get stuck in
the screen. Likewise, if the material contains straw, some straw may come to rest on the screen and
not pass through. Examine the mill after the milling is completed. If any such particles are found, grind
them manually until they pass the sieve and add this material to the sub-sample.
Spread out the sub-sample in a tray no more than a few millimetres deep and leave it for at least 4 h in
the laboratory until it reaches equilibrium with the temperature and humidity in the laboratory.
Material that has been subjected to the particle size-reduction processes described in this subclause
shall not be used for the determination of the total moisture content of the fuel.
NOTE 3 Sample division can be carried out between subsequent particle reduction steps as long as the

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minimum mass in Table 1 is respected.

9.7 Sample division of <1 mm material

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If required, e.g. for back-up samples, divide the <1 mm material into two or more sub-samples using
one of the methods described in Clause 8. It is strongly recommended to use division instead of simple
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extraction by scoop/spatula whenever possible.
If impurities (like sand, etc.) are expected, then care should be taken especially for the segregation of
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particles, so the use of sample dividers is recommended. The sub-samples for further grinding shall
keep the minimum masses stated in Table 2.

9.8 Particle size reduction of <1 mm material to <0,25 mm

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When a sub-sample is required with a nominal top size of 0,25 mm, use a cutting mill to reduce one
of the <1 mm sub-samples to this size. Feed the cutting mill with small portions of material from
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the <1 mm sub-sample and let each portion pass through the 0,25 mm screen to prevent excess heat
generation.
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NOTE Depending on the material, mills other than the cutting mill can be used.

10 Storage and labelling

Samples shall be placed in air-tight plastic containers or bags. Each sample shall be labelled with a
unique identification number of the sample, date and time of sampling and identification number or
code of the lot or sub-lot number.

11 Performance characteristics
Data regarding the uncertainty of this document have been acquired through the validation
investigation, these among others being the BioNorm projects. These results give information on
the uncertainty of the sample preparation and analysis. Results are presented in Annex A. For the
validated fuel types, these values can be used in combination with their own laboratory performance
characteristics and a desired coverage factor to get the overall uncertainty that is demanded.
The precision of the overall sampling shall be in accordance with ISO 18135.
Additionally, Annex B and Annex C are included to schematically communicate sample preparation for
samples from single deliveries and from continuous delivery applications.

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Annex A
(informative)

Precision in relation to division method

The referred results below were obtained in the research study of the EU projects BioNorm and
BioNorm2. The study was performed as repeatability experiments where the sample types in Table A.1
were divided into 16 sub-samples by the reduction methods coning and quartering, long pile, riffle box
and handful sampling with and without coarse cut, respectively. Each sub-sample was analysed for the
parameters in Tables A.2 to A.13 as single analyses. The investigation of sample types 1, 2, 6, 8, 9 and
10 was performed by a Swedish laboratory, sample types 3, 4 and 5 by an Italian laboratory and sample
type 7 by a Danish laboratory. The performance of the reduction methods was evaluated by comparison
of the coefficient of variance (CV,r) of the repeatability. Outliers were detected using the Dixon outlier
test. The riffle box used in Sweden had a total number of eight slots with a width of 45 mm each, while
the riffle box used in Italy had a total number of 16 slots and a slot width of 25 mm.

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Table A.1 — Description of solid biofuel materials
Nr. Sample type Sub-sample size Sample origin

1 Bark a
kg dry matter
1,5 ± 0,05
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Bark from Scots pine with a nominal top size of 100 mm
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2 Wood chipsa 0,5 ± 0,03 Wood chips from stem wood including bark with a nominal top
size of 16 mm. Conifer: Deciduous 95:5
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3 Olive residuea 0,5 ± 0,02 Olive residues (typical Mediterranean materials) with a nominal
top size of 3 mm
4 Grape residuea 0,5 ± 0,03 Grape residues (typical Mediterranean materials) with a nominal
top size of 16 mm
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5 Pellets (6 mm)a 0,9 ± 0,05 6 mm pellets produced from a whole deciduous tree
6 Stem wood 0,5 ± 0,03 8 mm pellets produced from stem wood including bark (see wood
pellets chips above)
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(8 mm)a
7 Wheat strawb 0,25 ± 0,01 Wheat straw in square bales
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8 Sawdustb 0,25 ± 0,02 Sawdust from conifer with a nominal top size of 5,6 mm
9 Logging resi- 1,0 ± 0,07 Logging residue from conifer including bark with a nominal top
dueb size of 64 mm
10 Pellets (8 mm)b 0,5 ± 0,05 8 mm pellets from sawdust of conifer
11 Palm kernel 0,029 ± 0,005 Palm kernel shell in 5 mm to 25 mm size available from the palm
shellsc oil milling process
a Materials investigated in BioNorm2.
b Materials investigated in BioNorm.
c Palm Oil Engineering Bulletin No. 70.

14  © ISO 2017 – All rights reserved

 Table A.2 — Performance data for moisture content (%)
Handful sampling Handful sampling
Coning and quartering Long pile Riffle box
without coarse cut with coarse cut
 

Sample l o xm CV,r l o xm CV,r l o xm CV,r l o xm CV,r l o xm CV,r

type
1
2
16 0 54,2 0,57 16 0 56,2 0,59

3
16 0 48,40 0,30 16 0 49,5 0,34 15 6 50,38 0,23

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14 12 5,33 0,79 16 0 10,7 0,30 14 12 4,91 1,6

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16 0 62,4 2,3 16 0 56,9 1,2 16 0 56,6 1,1
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16 0 15,6 0,74 16 0 S
15,5 1,0 16 0 16,0 1,8 16 0 15,3 1,8

9
16 0 55,2 0,47 15 6 54,8 0,45 16 0 55,6 0,52

10
16 0 51,2 0,64 16 0 51,8 0,95 16 0 51,8 0,54

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16 0 5,67a 0,48a 15 6 5,49
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0,77 16 0 5,45 0,64
5 0 12,0 1.1
a For sample type 10, a rotary divider was used instead of coning and quartering.


l       number of outlier-free individual analytical values per level
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o      percentage of outlying values from the replicate determinations
xm    overall mean in %
CV,r   coefficient of the variation of the replicates
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Table A.3 — Performance data for ash content (%)

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Handful sampling Handful sampling
Coning and quartering Long pile Riffle box
without coarse cut with coarse cut
Sample l o xm CV,r l o xm CV,r l o xm CV,r l o xm CV,r l o xm CV,r
type
1
2
ISO 14780:2017(E)

16 0 6,53 6,3 16 0 7,60 4,8

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16 6 0,59 7,8 14 0 0,77 2,6 16 0 0,74 2,4

4
16 0 9,5 34,1 16 0 10,2 37,7 16 0 10,5 22,7

5
16 0 6,60 8,1 16 0 7,02 9,1 16 0 7,98 10,0a

6
16 0 0,61 21,8 16 0 0,54 35,9 16 0 0,47 17,1

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16 0 0,36 5,2 16 0 0,34 6,8 16 0 0,34 4,4
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8
9
16
16
0
0
4,9
0,29
4,7
8,8
16
16
0
0
4,1
0,28
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10,5 16 0 0,39 13,0
16 0 4,2 4,6 16 0 4,2 3,5

10
16 0 2,9 13,8 16 0 3,1 10,3 16 0 3,3 9,7

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16 0 0,30b 0,023b 16 0 0,34 6,6 U 16 0 0,34 2,4


5 0 3,0 1,3
a Grape material is sticky. This negatively influences the performance of the riffle box.
b For sample type 10, a rotary divider was used instead of coning and quartering.
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Table A.4 — Performance data for calorific value (MJ/kg)

Coning and quartering Long pile
Sample l o xm CV,r l o xm CV,r
type
1 16 0 20,00 0,45 16 0 19,77 0,37

Table A.5 — Performance data for mechanical durability (%)

  Coning and quartering Long pile Riffle box
Sample l o xm CV,r l o xm CV,r l o xm CV,r
type
5 16 0 96,4 0,30 16 0 96,4 0,16 14 12 96,6 0,12
6 15 6 96,7 0,13 15 6 96,8 0,10 16 0 96,9 0,13

Table A.6 — Performance data for potassium content (mg/kg)

  Coning and quartering Long pile Riffle box

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Sample l o xm CV,r l o xm CV,r l o xm CV,r
type
3 16 0 5 254 17 16 0 7 973 16 16 0 6 573 28
4 16 0 15 727 17 16 0 N 23 414 8 16 0 20 251 15
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Table A.7 — Performance data for nitrogen content (%)
  Coning and quartering Long pile Riffle box
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Sample l o xm CV,r l o xm CV,r l o xm CV,r

type
3 16 0 1,28 39,7 16 0 1,55 38,3 16 0 0,83 40,4
4 16 0 2,36 13,3 15 6 2,70 5,4 14 12 2,56 13,8
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Table A.8 — Performance data for particle size distribution  >8 mm to <16 mm (%)
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  Coning and quartering Long pile Riffle box

Sample l o xm CV,r l o xm CV,r l o xm CV,r
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type
2 16 0 13,7 6,8 16 0 14,0 7,8 16 0 12,3 7,1

Table A.9 — Performance data for particle size distribution  >5 mm to <8 mm (%)
  Coning and quartering Long pile Riffle box
Sample l o xm CV,r l o xm CV,r l o xm CV,r
type
2 16 0 35,6 2,2 16 0 36,1 1,6 15 6 34,3 1,1

Table A.10 — Performance data for particle size distribution  >3 mm to <5 mm (%)
  Coning and quartering Long pile Riffle box
Sample l o xm CV,r l o xm CV,r l o xm CV,r
type
2 16 0 32,5 2,7 16 0 31,3 2,4 16 0 33,1 2,2

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ISO 14780:2017(E)


Table A.11 — Performance data for particle size distribution  >2 mm to <3 mm (%)
  Coning and quartering Long pile Riffle box
Sample l o xm CV,r l o xm CV,r l o xm CV,r
type
2 16 0 8,0 5,6 16 0 7,8 5,9 16 0 8,4 3,2

Table A.12 — Performance data for particle size distribution <2 mm (%)

  Coning and quartering Long pile Riffle box
Sample l o xm CV,r l o xm CV,r l o xm CV,r
type
2 16 0 9,7 4,0 16 0 10,2 5,5 16 0 11,0 3,2

Table A.13 — Performance data for chloride content (%)

  Coning and quarter- Handful sampling Handful sampling
Long pile
ing without coarse cut with coarse cut

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Sample l o xm CV,r l o xm CV,r l o xm CV,r l o xm CV,r
type
7 16 0 0,397 1,5 16 0 0,404 2,0 16 0 0,391 2,7 16 0 0,389 1,5
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Annex B
(informative)

Scheme of sample preparation for samples from single delivery

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Annex C
(informative)

Scheme of sample preparation for samples from continuous

delivery

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Bibliography

[1] ISO 13909 (all parts), Hard coal and coke — Mechanical sampling
[2] ISO 18283, Hard coal and coke — Manual sampling
[3] EN 14780, Solid Biofuels — Sample Preparation
[4] BIONORM II Pre-normative work on sampling and testing of solid biofuels for the development
of quality management, EU-project 038644, project coordinator Kaltschmidt M., final report
Leipzig 11.1.2011

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ICS 27.190; 75.160.40
Price based on 22 pages

© ISO 2017 – All rights reserved