Solid recovered fuels - Methods for the determination of ash melting behaviour by using characteristic temperatures

This Technical Report describes exemplarily methods for the determination of shrinking, deformation, hemisphere and flow temperature for characterising the ash melting behaviour of all solid recovered fuels.

Feste Sekundärbrennstoffe - Verfahren zur Bestimmung des Schmelzverhaltens der Asche bei Anwendung charakteristischer Temperaturen

Dieser Fachbericht beschreibt beispielhaft Verfahren zur Bestimmung der Schrumpfungs-, Erweichungs-,
Halbkugel- und Fließtemperatur zur Charakterisierung des Schmelzverhaltens der Asche von festen Sekundärbrennstoffen.

Combustibles solides de récupération - Méthode de détermination de la fusibilité des cendres

Trdna alternativna goriva - Metode za določevanje karakterističnih temperatur tališča pepela

To tehnično poročilo opisuje vzorčne metode za določevanje krčenja, deformacije, hemisfere in dotočne temperature za karakterizacijo tališča pepela vseh trdnih alternativnih goriv.

General Information

Status
Published
Publication Date
07-Sep-2010
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Start Date
08-Sep-2010
Due Date
01-Oct-2010
Completion Date
08-Sep-2010

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SLOVENSKI STANDARD
01-november-2010
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SIST-TS CEN/TS 15404:2007
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Solid recovered fuels - Methods for the determination of ash melting behaviour by using
characteristic temperatures
Feste Sekundärbrennstoffe - Verfahren zur Bestimmung des Schmelzverhaltens der
Asche bei Anwendung charakteristischer Temperaturen
Combustibles solides de récupération - Méthode de détermination de la fusibilité des
cendres
Ta slovenski standard je istoveten z: CEN/TR 15404:2010
ICS:
75.160.10 Trda goriva Solid fuels
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

TECHNICAL REPORT
CEN/TR 15404
RAPPORT TECHNIQUE
TECHNISCHER BERICHT
September 2010
ICS 75.160.10 Supersedes CEN/TS 15404:2006
English Version
Solid recovered fuels - Methods for the determination of ash
melting behaviour by using characteristic temperatures
Combustibles solides de récupération - Méthode de Feste Sekundärbrennstoffe - Verfahren zur Bestimmung
détermination de la fusibilité des cendres des Schmelzverhaltens der Asche bei Anwendung
charakteristischer Temperaturen

This Technical Report was approved by CEN on 12 June 2010. It has been drawn up by the Technical Committee CEN/TC 343.

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
© 2010 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TR 15404:2010: E
worldwide for CEN national Members.

Contents Page
Foreword .3
Introduction .4
1 Scope .5
2 Normative references .5
3 Terms and definitions .5
4 Principle .6
5 Reagents .6
6 Apparatus and auxiliary means .6
7 Test conditions .7
8 Methodology .8
9 Procedure .8
10 Evaluation of available results .9
Annex A (informative) Interlaboratory test results . 12
Bibliography . 17

Foreword
This document (CEN/TR 15404:2010) has been prepared by Technical Committee CEN/TC 343 “Solid
recovered fuels”, the secretariat of which is held by SFS.
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 supersedes CEN/TS 15404:2006.
CEN/TS 15404:2006 was not to be kept as a Technical Specification and respectively not converted into a
European Standard due to lack of acceptable precision data (see [1], [2]).
This document differs from CEN/TS 15404:2006 as follows:
a) symbol of shrinking temperature changed from ST to SST;
b) charts and key of Figure 1 corrected;
c) clause "Precision" deleted;
d) clause on evaluation of results added;
e) interlaboratory test results supplemented as graphs in an informative annex;
f) whole document editorially revised.
Introduction
Ash melting is a complex process where also shrinkage, sintering and swelling can occur.
The test methods described in this Technical Report provide information about fusion and melting behaviour
of the composite inorganic constituents of the fuel ash at high temperatures.
The test methods available are empirical in most cases. The ashes used for the tests are homogeneous
material, prepared from the fuel, and the determination is performed at a controlled rate of heating in a
controlled atmosphere. In contrast, under full-scale conditions, the complex processes of combustion and
fusion involve heterogeneous mixtures of particles, variable heating rates and gas compositions.
The methods described in this document should be used dependent of the following aspects and parameters,
respectively:
 repeatability;
 reproducibility;
 reliability;
 time efforts (rapid test methods);
 cost effectiveness;
 possibilities for automatic testing.
The aim of this document consists in providing a common and successful practice for describing the ash
melting behaviour.
The terms ash fusibility and ash softening are synonyms to ash melting.
1 Scope
This Technical Report describes exemplarily methods for the determination of shrinking, deformation,
hemisphere and flow temperature for characterising the ash melting behaviour of all solid recovered fuels.
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.
prEN 15357:2008, Solid recovered fuels — Terminology, definitions and descriptions
prEN 15403, Solid recovered fuels — Determination of ash content
ISO 3310-1, Test sieves — Technical requirements and testing — Part 1: Test sieves of metal wire cloth
3 Terms and definitions
For the purposes of this document, the terms and definitions given in prEN 15357:2008 and the following
apply.
3.1
shrinking temperature
SST
temperature at which shrinking of the test piece occurs, i.e. when the area of the test piece falls below 95 % of
the original test piece area at 550 °C
NOTE Shrinking can be due to liberation of carbon dioxide, volatile alkali compounds, and/or sintering and partial
melting.
3.2
deformation temperature
DT
temperature at which the first signs of roundings of the edges due to melting of the test piece occur
3.3
hemisphere temperature
HT
temperature at which the test piece forms approximately a hemisphere, i.e. when the height becomes equal to
half the base diameter
3.4
flow temperature
FT
temperature at which the ash is spread out over the supporting tile in a layer, the height of which as half of the
height of the test piece at the hemisphere temperature
NOTE Half of the height of the test piece is defined due to frequently occurring bubbling effects. This is especially
important for automatic image evaluation. This definition is different to other standards.
4 Principle
A test piece made from the prepared ash is heated up with constant rate whereas the deformation is
continuously observed. The temperatures at which characteristic changes of the shape occur are recorded.
5 Reagents
5.1 Water, demineralised.
5.2 Dextrin, 100g/l solution: 10 g of dextrin are dissolved in 100 ml water.
5.3 Ethanol, with a purity of greater than 95 %.
5.4 Carbon dioxide
5.5 Gas mixture, of carbon dioxide (5.4) and carbon monoxide: A volume fraction of 55 % to 65 % carbon
monoxide is mixed with a volume fraction of 35 % to 45 % carbon dioxide (5.4).
5.6 Gold wire, with a diameter of 0,5 mm or greater, or a gold plate, with a thickness of 0,5 mm to 1,0 mm,
a purity of at least 99,99 % and a certified melting point (e.g. 1 064 °C).
5.7 Nickel wire, with a diameter of 0,5 mm or greater, or a nickel plate, with a thickness of 0,5 mm to
1,0 mm, a purity of at least 99,9 % and a certified melting point (e.g. 1 455 °C).
NOTE Nickel is used for reducing atmosphere.
5.8 Palladium wire, with a diameter of 0,5 mm or greater, or a palladium plate, with a thickness of 0,5 mm
to 1,0 mm, a purity of at least 99,9 % and a certified melting point (e.g. 1 554 °C).
6 Apparatus and auxiliary means
6.1 Furnace, electrically heated, capable to:
a) reach the maximum temperature (≥ 1 500 °C) at which the properties of the ash shall be determined;
b) provide and maintain an adequate zone of uniform temperature which to heat the test piece(s) in;
c) provide means for heating the test piece(s) at an uniform rate from 550 °C upwards;
d) maintain the required test atmosphere around the test piece(s);
e) provide means for observing the change of shape of the test piece(s) during heating.
6.2 Dish, consisting of inert material, such as porcelain, silica, platinum, with a depth from 10 mm to 20 mm
and of such a size that the sample loading does not exceed 0,1 g/cm bottom area.
6.3 Pyrometer, consisting of a platinum/platinum-rhodium thermocouple.
6.4 Mould, of brass, stainless steel or other suitable material for preparing the test piece.
6.5 Spring pressure hand press for producing the test piece, capable of providing a spring pressure of
about 1,5 N/mm .
6.6 Support for the test piece, consisting of such an inert material that it neither is distorted nor absorbs the
ash during the determination.
NOTE Supports of sintered alumina or fine-textured mullite are generally satisfactory but difficulties can arise with
individual ashes, in which case a non-absorbent interface such as platinum foil can be used between the original support
and the test piece.
6.7 Flowmeters, two, for measuring the components of the reducing gases.
NOTE If using oxidising gas, it is not necessary to measure the flow rate.
6.8 Grinding device, such as agate mortar and pestle.
6.9 Test sieve, of aperture 0,075 mm and diameter of at least 100 mm complete with lid and receiver, in
accordance with ISO 3310-1.
6.10 Optical instrument, such as a camera or video equipment, for observing the profile of the test piece
throughout the determination.
7 Test conditions
7.1 Test atmosphere
Oxidising or reducing atmosphere is used depending on the application. Air or carbon dioxide is applied for an
oxidising atmosphere. For a reduced atmosphere, the following mixtures shall be passing the test piece at a
minimum linear rate of flow from 100 mm/min to 250 mm/min calculated at ambient temperature:
 55 % volume fraction to 65 % volume fraction carbon monoxide with 35 % volume fraction to 45 %
volume fraction carbon dioxide, and
 45 % volume fraction to 55 % volume fraction hydrogen with 45 % volume fraction to 55 % volume
fraction carbon dioxide.
NOTE The flow rate is not very critical, provided that it is sufficient to prevent any leakage of air into the furnace in
case of reducing atmosphere. However, the same flow rate level is also recommended for oxidising atmosphere. For
open-type furnaces with a larger diameter, a flow rate of about 400 mm/min could be needed for reducing atmosphere. In
all cases it should also be referred to manufacturer instructions. The flow rate for rotameter adjustment can be calculated
by multiplying the flow rate, expressed in millimetres per minute, with the inside cross-section area of the furnace tube
converting into litres per minute.
WARNING — When using reduced atmosphere as given above, the gases emerging from the furnace
will contain a proportion of carbon monoxide; therefore it is essential to ensure that these gases are
vented to the outside atmosphere, preferably by means of a hood or an efficient fan system. If
hydrogen is used in the reducing atmosphere, care shall be taken to prevent an explosion occurring
by purging with carbon dioxide both prior to the introduction of the hydrogen and after the hydrogen
supply is shut off.
7.2 Shape of test piece
The test piece shall have sharp edges to facilitate observation.
The mass of the test piece shall be such as to ensure equalisation of the temperature within the test piece.
Hence, dimensions that are too large shall be avoided. Several test piece shapes are used, e.g. cylinders,
pyramids, cubes, truncated pyramids, with dimensions (diameter or height) in the vicinity of 3 mm to 5 mm.
Figure 1 illustrates a cylindrical shape test piece at the various characteristic temperatures.
Key
1 original sample
2 sample at shrinkage temperature
3 sample at deformation temperature
4 sample at hemisphere temperature
5 sample at flow temperature
Figure 1 — Phases in the ash melting process (original shape == shape and size at 550 °C)
==
8 Methodology
The ash shall be prepared in accordance
...

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