Page 1 of 26
Using used tyres as an alternative
source of fuel
Reference values and
characterisation protocols
Copyright Aliapur 2009
Reference document
July 2009
R&D Department
U
Using used tyres as sources of fuel – reference values and characterisation protocols
© Copyright Aliapur – R&D – July 2009
Page 2 of 26
In the first part of the present document, there is a presentation of the “reference
values” established by Aliapur on the basis of analyses carried out in 2007 and 2008
on several representative samples of the arising of used tyres, with regard to the
most relevant physical and chemical parameters for using tyres as fuel: heat output
and the fundamental composition of tyres. These reference values are made
available to industries that utilise used tyres as fuel to help them calculate and
declare their CO2 emissions in the context of the National Allocation Plan of CO2
allowances1.
This work was the opportunity to position used tyres as one of the main other sources
of traditional solid fuels.
In addition, in the second part, this work presents the particularities of the
characterisation protocol for the tyres and the analyses of the various physical and
chemical parameters (and, in particular, the biomass fraction of used tyres).
This document has thus been produced for both industrialists who use used tyres, as
well as the Administration, in the context of the dispensation accorded by the
MEEDDAT (the French state department for the ecology, energy, sustainable
development and land use) on the use of a default value for the biomass fraction for
used tyres in the calculation of CO2 emissions.
1
A decree dated 31 March 2008 concerning the verification and quantification of emissions declared
in the context of the European greenhouse gas emissions trading scheme for the period 2008-2012.
Using used tyres as sources of fuel – reference values and characterisation protocols
© Copyright Aliapur – R&D – July 2009
Page 3 of 26
Document written with the assistance of
CONTENTS
Introduction and context................................................................................... 4
I.
Reference values .......................................................................................... 6
A. Spotlight on the key parameters ..................................................................... 7
B. Comparison with other solid fossil fuels ....................................................... 7
C. Values for the other elements in the fundamental composition .................. 9
II. Characterisation protocol for used tyres ........................................... 10
A. Used tyres: a homogenous product in terms of their uses… .................... 11
B. The different stages in the sampling protocol: taking and preparing the
sample.................................................................................................................. 12
1.
Simplified sampling protocol diagram ............................................................
2.
Detailed protocol – the constraints and requirements for each stage
12
................. 13
C. The analysis methods specific to used tyres .............................................. 15
D. The particular case of analysing the biomass fraction of tyres ................. 17
III. Appendices ................................................................................................... 18
Appendix I: Bibliographical sources ................................................................. 18
Appendix II: Excerpt from the circular dated 01 July 2008 from the
MEEDDAT – dispensation granted for evaluating the biomass fraction of
tyres ..................................................................................................................... 18
Appendix III: Detailed analysis methods for the different phases .................. 19
Appendix IV: Results of analyses methods on the elementary composition
of Passenger car and Truck ELT ....................................................................... 24
Appendix V: Detailed analysis results for 10 batches of shredded used
tyres ..................................................................................................................... 25
Using used tyres as sources of fuel – reference values and characterisation protocols
© Copyright Aliapur – R&D – July 2009
Page 4 of 26
Introduction and context
In the face of various new regulatory contexts and the importance of sustainable
development, the used tyre recycling sector has become organised so as to be able to codify
and harmonise its activities and provide homogenous products in terms of quality (format, cut
quality and composition).
Standardisation of characterisation methods and specific analyses for used
tyres has played a part in changing their status from waste to product.
At the French level, a standardisation committee (CN-PUNR-AFNOR2) focusing on the
products made from ELT (end-of-life tyres) has been working since 2005 on establishing
experimental standards so as to have common measurement and sampling methods3.
With the AFNOR standards that have already been published, France is currently the
most advanced European country in terms of standardisation of the products obtained
from ELT: French works are proposed as the work basis for defining European
standards.
A similar approach to standardisation of common methods for analysing solid recovered
fuels is currently under way at the European level (TC 343) and should result in the
publication of a proposed standard by the end of 2008.
In this context, Aliapur is highly involved in the works conducted by the committees of
the European Committee for Standardization for used tyres: in this context, and in
particular in terms of solid recovered fuel, Aliapur has had tested on its products all the
methods proposed by the TC343 work group and has been able to show that some of
these methods might have limitations when applied to shredded tyres.
→
The implementation of a characterisation protocol and analysis methods
specific to ELT is thus an essential step.
2
5 groups of experts have been created, including a group on tyre shredding, which works in particular on sampling shredded
stock of ELT, the preparations for analysis of the chemical composition of the sample and the analysis methods for the chemical
composition, and a liaison group for the technical committee on solid recovered fuels.
3
AFNOR XP T47-751: End-of-Life Tyres (ELT) - Determination of the format of products from primary shredding - Manual
method based on the measurement of the largest projected length
AFNOR XP T47-753: End-of-Life Tyres (ELT) - End-of-life tyres (ELT) - Determination of the format of products from primary
shredding – Method based on the automated measurement of the largest projected length
Determination of the particle size analysis of granulates issued from End-of-Life Tyres - Method based on the mechanical
sieving of product.
AFNOR XP T47-756: End of life tyres (ELT) - Sampling of products from primary shredding - Conveyor scenario
AFNOR XP T47-757: End-of-life tyres (ELT) – Determination of the format of products from primary shredding – Protruding wire
evaluation method
Using used tyres as sources of fuel – reference values and characterisation protocols
© Copyright Aliapur – R&D – July 2009
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Different regulatory requirements imposed on industries that use ELT need
specification of the protocol for characterising tyres and conducting physical
and chemical analyses. They also need to have reference values at their
disposal.
Certain industries, such as cement works and boiler rooms,
reduce their consumption of traditional fuels and thus also
Used tyres have the advantage of presenting not only a high
of traditional solid fuels (coke and coal), but also renewable
should not be neglected.
use ELT as fuel so as to
reduce their energy bills.
NCV that is similar to that
and mineral fractions that
Since the implementation of the National Allocation Plan of CO2 allowances in France4,
industrialists have been subject to new regulatory requirements that impose calculating
and declaring their CO2 emissions (including those associated with the combustion of
ELT) every year to the Authorities.
Depending on the level of emissions for these sites, and of the relative importance that
tyres can represent in relation to other sources of emissions, industrialists must calculate
their CO2 emissions using the following parameters, determined with a method level5
that is more or less high: quantity of fuel, NCV and emission factor (carbon content,
taking into account any possible biomass fraction). Depending on the level of emissions
on the site and the status of tyres among the other fuels used (major, minor or marginal
flow), industrialists must use either default values or specific values obtained from
analyses carried out by an ISO 17025:2005 certified laboratory, whilst respecting the
requirements in terms of sampling method and frequency of analysis6.
A general dispensation was granted by the MEEDDAT for the biomass fraction of ELT7
for 2008 and authorises operators to use a default value rather than carry out specific
analyses for the biomass fraction, regardless of the category of tyre (major, minor or
marginal). This value was established by the MEEDDAT on the basis of the initial data
provided by Aliapur in 2007 on the concentration in natural rubber (the MEEDDAT
retained 14.6 % of natural rubber for average tyres – see Appendix I).
In accordance with the European Directive, this dispensation must nevertheless be reevaluated at the national level every year.
→
Given the new elements provided by the results of studies and analyses
conducted on the initiative of Aliapur in 2008, Aliapur considers that it is
necessary to provide additional information on this subject.
4
PNAQ established by France for the period 2005-2007 (PNAQ 1), then 2008-2012 (PNAQ 2) following the
European Directive known as the Quotas Directive : 2003/87/EC
5
The method level defines: on the one hand, the expected precision of the activity variables (that is, the
quantities of fuel consumed (a “performance obligation”) and, on the other, the requirements in terms of
sampling and measuring emission and oxidation factors and the NCV (an “obligation of means”).
6
Excerpt from the decree of 31 March 2008 (annex I, §III-3): “The operator must provide proof that the samples
obtained are representative and exempt of bias. The respective value must only be used for the delivery period or
the batch of fuel or materials of which it is representative. […] The sampling procedure and frequency of
analysis must make it possible to guarantee that the annual average for the parameter in question be determined
with maximum uncertainty that is less than one third of the maximum uncertainty required by the method level
approved for the activity data concerning the same flow.” If if it impossible for the operator to meet this
requirement, minimal frequency of analysis are provided in the decree.
7
Appendix II of the Circular dated 1 July 2008
Using used tyres as sources of fuel – reference values and characterisation protocols
© Copyright Aliapur – R&D – July 2009
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I. Reference values
The reference values presented in the present document were obtained from the results of
analyses carried out in the laboratory on 8 samples of shredded ELT (5 samples from
production and 3 samples from loading the barge).
In order to take into account the heterogeneity of the tyres at the microscopic level, it is
necessary to either take a large number of samples, or a smaller number but with
preparation work. Given the number of characteristics to be analysed (more than 35), the
second option was chosen at Aliapur.
The samples were obtained in accordance with standard XP T47-756: End of life tyres (ELT)
- sampling of products from primary shredding - Conveyor scenario.
They were composed of 3 samples taken
→ from the material flow, from under the conveyor belt during production of batches of
20 to 250 tonnes (for samples on the shredding site, representing between 1 day and
2 weeks of production)
→ during loading / unloading of the barges of 1,500 to 2,500 tonnes.
The shredded material came from:
→ mainly End-of-Life Tyres from Passenger cars (PC)
→ mainly End-of-Life Tyres from Trucks.
The localisation of the various zones from which the quantities of samples were obtained is
presented on the map below.
Samples taken and analysed by Aliapur in 2007/2008
Samples taken and
analysed by Aliapur in
2007/2008
The results showed that there was good coherence and consistency with the nature of the
tyres. The shredded material contained more than 90 % of carbon, iron, hydrogen, oxygen,
silica, zinc and sulphur.
Using used tyres as sources of fuel – reference values and characterisation protocols
© Copyright Aliapur – R&D – July 2009
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A. Spotlight on the key parameters
Passenger car ELT
Min
Max
Average
Truck ELT
Min
Max
Average
NCV (MJ/kg)
29.5
30.6
30.2
26.1
26.7
26.4
Carbon (C)
67.5%
70.1%
69.0%
59.7%
62.6%
61.1%
Biomass fraction
17.0%
20.3%
18.3%
28.6%
29.7%
29.1%
1.2%
1.4%
1.3%
1.2%
1.6%
1.4%
(% mass)
Sulphur (S)
The values come from analyses carried out on 8 samples for passenger cars and 2 samples
for trucks (the detailed results for each sample are presented in Appendix V).
The results of the analyses carried out on the tyre samples, representative of the generation
of ELT in France, showed little variability in terms of NCV, C, C biomass and sulphur
parameters.
The truck used tyres have NCV and carbon contents that are lower than those of passenger
cars because of the higher proportion of metal in the tyres. Conversely, the content in carbon
of biomass origin is greater in the case of used truck tyres.
B. Comparison with other solid fossil fuels
Passenger car
ELT
Truck
NCV (MJ/kg)
30.2
Carbon (C)
Coal
Petroleum coke
26.4
26
32
69%
61%
64-68%
84-97%
18.3%
29.1%
0%
0%
Sulphur
1.3%
1.4%
1.3%
0.2-6%
EF: t CO2/TJ
59 (x)
43 (x)
90-95*
96*-110
EF: t CO2/t
1.8 (x)
1.1 (x)
2.5
3.1
Biomass fraction
ELT
(% mass)
* Default values for Emission factors (EF) of Coal and coke quoted in the 31 March 2008 decree
12
** TJ = 10 joules (tera joules)
(x) Net emission factors, taking the biomass carbon into account.
Using used tyres as sources of fuel – reference values and characterisation protocols
© Copyright Aliapur – R&D – July 2009
Page 8 of 26
Used tyres used as fuel have a high heating value that varies little in relation to the samples
taken from the trucks and passenger cars arising, and it is comparable with that of coal and
petroleum coke.
In addition, the particularity of ELT is their low sulphur content (around 1.3%, equivalent to
that of coal) in comparison with sulphur content for petroleum coke which can vary
considerably depending on the origin of the fuel, reaching as much as 6% and thus requiring
air pollution control (to reduce the SO2 emissions so as to respect the emission limit values).
Given the analysis elements for the NCV, carbon content and biomass, the emissions factor
for ELT calculated was around 59 t CO2 / TJ for passenger car used tyres and 43 t CO2 /TJ
for the truck used tyres, or 45% less than that of petroleum coke and coal.
Tyres thus make it possible not only to provide a heat output equivalent to that
of petroleum coke and coal, but also make it possible to reduce fossil CO2
emissions due to combustion significantly because of their biomass fraction
(up to 45% of the fuel emissions in case of 100% substitution of coke by used
tyres).
Thus, if we take as an example the production of one tonne of clinker (at the level of a
furnace of average consumption of 3,300 MJ/t of clinker the combustion emissions were as
follows depending on the fuel mix:
Fuel mix
Fuel flow
Combustion
emissions
(kg CO2 / t ck)
100% petroleum coke
0.1 t coke
314 kg CO2 / t ck
100% coal
0.13 t coal
317 kg CO2 / t ck
100%
tyres
passenger
car 0.11 t passenger car 194 kg CO2 / t ck
ELT
xxx
Fossil CO2
emission
reduction*
-38%
xxxxxxxxxxxxx
142 kg CO2 / t ck
-55%
174 kg CO2 / t ck
-45%
50% coke + 50% 0.05 t coke + 0.05 t
passenger car ELT
passenger cars
255 kg CO2 / t ck
-19%
100% truck tyres
0.12 t truck ELT
100% used tyres
0.11 t tyres
(70% passenger car +
30% Truck)8
* Reduction calculated in relation to the average value for 100% coke or 100% coal
8
Distribution of the tyres on the market in 2007, taken from the ADEME report on the 2007 data for tyres
(Synthèse Données 2007 pneus – collection Repères): the distribution between passenger car tyres (passenger
cars tyres of less than 15 kg) and truck tyres (more than 15 kg) was 70% / 30%.
Using used tyres as sources of fuel – reference values and characterisation protocols
© Copyright Aliapur – R&D – July 2009
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C. Values for the other elements in the fundamental composition
Used tyres have a carbon content of more than 60%, up to 70% for passenger car tyres.
One of the particularities of used tyres is their composition in iron that is also a major element
as it can represent up to 27% of the composition of truck tyres. This source of iron is,
furthermore, recycled by cement makers (on the condition however that the output remains
compatible with the global balance at the clinker and cement level).
Content in % mass
Major elements (>1%)
Passenger car
Truck
Coal
Petroleum coke
Carbon (C)
68 to 70%
60 to 63%
63.9%
84 to 97%
Iron (Fe)
11 to 12%
25 to 27%
Hydrogen (H)
6 to 6.3%
5.3 to 5.6%
Oxygen (O)
3.3 to 3.8%
1.5 to 2.2%
Silica (Si)
1.5 to 1.9%
0.3 to 0.5%
Zinc (Zn)
1.3 to 1.5%
1.3 to 1.8%
Sulphur (S)
1 to 1.5%
0 to 0.2%
3.6%
0 to 5%
2%
Nd
1.2 to 1.6%
1.3%
0.2 to 6%
Passenger car
Truck
Coal
Petroleum coke
Nitrogen (N)
0.4 to 0.6%
0.3 to 0.4%
1.3 to 1.8%
1.5 to 2%
Calcium (Ca)
0.2 to 0.3%
0.06 to 0.08%
0.18%
Nd
Manganese (Mn)
0.06 to 0.07%
0.1 to 0.2%
0.1%
Nd
Minor elements (<1%)
The following elements were present at a concentration of < 0.06% (trace elements) (see
Appendix IV):
aluminium, arsenic, barium, bromide, chloride, chrome, cobalt, copper, magnesium,
molybdenum, nickel, phosphorous, lead, potassium, sodium, titanium.
Nickel in particular was present at a concentration ranging from 0.002 to 0.003%.
The other elements present at concentrations of < 0.001% (at the quantification limit) were:
selenium, antimony, beryllium, vanadium and mercury were
The elements present at concentrations of < 0.002% (quantification limit) were:
fluorine, cadmium and thallium
Using used tyres as sources of fuel – reference values and characterisation protocols
© Copyright Aliapur – R&D – July 2009
Page 10 of 26
II. Characterisation protocol for used tyres
Summary
Aliapur has carried out a range of studies with the BRGM, SGS, CTTM, BETA and the
LRCCP, which have shown that it is not always possible to analyse used tyres with the
methods designed for other solid recovered fuels.
Aliapur has thus defined and proposed, particularly in the context of the work of the TC343, a
protocol and specific analysis methods for characterising tyres that make it possible to:
- let the intrinsic heterogeneity of tyres be expressed during the sampling, sample
preparation and test sample stages
- do the preparation and sampling without resulting in either loss, nor addition nor chemical
alteration of the material
- analyse the various parameters without bias.
The operating procedure for preparing samples makes it possible to isolate three distinct
phases, the presentation of which makes it possible to perform representative analyses
(homogenous matter).
It must be monitored strictly so as to know the exact distribution of each phase and to be
able to ultimately establish the chemical composition of the sample.
Finally, the analysis methods must be adapted to the characteristics of the different phases.
This operating procedure for sampling and analysis is the procedure that has been used by
Aliapur to establish the reference data presented in the first part of this document.
Using used tyres as sources of fuel – reference values and characterisation protocols
© Copyright Aliapur – R&D – July 2009
Page 11 of 26
A. Used tyres: a homogenous product in terms of their uses…
…but which are heterogeneous at the microscopic level, requiring precautions
in the pre-analysis preparation
The products obtained from recycling are often qualified as heterogeneous. And there is,
indeed, an intrinsic heterogeneity to ELT, at the microscopic level, related to their
composition.
TYRES
Tyres are effectively composite materials,
essentially made of elastomers, metal wire
and textile fibres. These components are,
in addition, different depending on the part
of the tyre in which they are used. For
example, elastomer mixtures are not the
same in the various parts of the tyre.
Tread block
Grooves
and sipes
Sidewall
Belt
Inner
liner
Bead insulation
and bead
Insulation
Bead
This microscopic heterogeneity is of importance, and must be taken into consideration for
the analyses, but does not appear at the scale of industrial use (consumption of around one
tonne an hour). This is why the physical and chemical characteristics measured within an
arising of ELT do not show any particular heterogeneity.
Certain occasional analyses do not correctly take into account the notions of sampling
strategy and preparation of test samples. The results of these analyses have, as a result,
obtained very different values for a single product. This nevertheless does not mean that the
physical and chemical parameters representative of a tonne of tyres present significant
variability. The results obtained under sample, test and analysis conditions respecting good
practices with regards to heterogeneous materials show, on the contrary, remarkable
stability in the parameters measured (see the results of the batch analyses used to establish
the reference values, presented in the Appendix).
The solution for determining, with some precision, the composition in a given quantity of a
batch of material from a sample goes through an optimal number of sample takings, to
define a statistical approach (either a large number of samples, or a smaller number with
pre-analysis preparation work).
Taking a sample from a heterogeneous material is effectively a random process, producing
the sampling errors that are listed below and that need to be reduced via preparation work:
→ errors of preparation and sampling: the result in particular of the loss or addition of
matter, or chemical alteration
→ errors of segregation, caused by the heterogeneity of distribution9: this error can be
virtually cancelled out in cases of homogenisation of the batch by mixing, or by
carrying out a maximum number of elementary samples on all of the material by
means of quartering, for example
→ fundamental sampling errors, related to the heterogeneity of composition10, and
perhaps limited if all the particles have an equal chance of being taken in a sample.
9
The heterogeneity of distribution essentially results from spatial, non random distribution of particles within a batch. It depends
on the size of the particle groups on which the observations are made, and also on the heterogeneity of the composition of the
material studied (see below).
10
The heterogeneity of composition results from the frequency and physical and chemical particularities of the individual
particles in the matter and is exclusively related to the intrinsic properties (chemical composition, size, mass…) of each
individual element of the material and is independent of their spatial distribution.
Using used tyres as sources of fuel – reference values and characterisation protocols
© Copyright Aliapur – R&D – July 2009
Page 12 of 26
B. The different stages in the sampling protocol: taking and
preparing the sample
The aim of the protocol developed by Aliapur is to make it possible to reliably determine the
content in chemical elements of samples of used tyres. The samples must, in addition, be
representative of the arising studied.
1. Simplified sampling protocol diagram
The following diagram summarises the sequence of the different stages of the ELT
characterisation protocol, starting with the sampling of ELT, to the preparation of the sample,
the test sample, to the various methods of specific analysis, and this, for each phase.
Sampling – Taking the sample
Prélèvement
– Prise d’échantillon
Sampling
Prélèvement
d’incrément
Sampling
of increment
représentatif
representative
of at d’au
leastmoins 20t
20 t
Flow
of ELTprélevé:
material sampled:
Flux
de matière
→cours
Fromdeproduction
on site
thede
shredding
- En
production sur
site (batches
ofà20
broyage
(lots de 20
150tot)150t)
→cours
Fromduthe
loading process
- Au
chargement
de barge into the
barge
(batches
(lots
de 1500
à 2500of
t) 1,500 to 2,500t)
T 47 - 756
Standards
Norme XP T47-756
Reduction
Réduction by
par quartering
quartage
25
kgmaximum
maximum
25 kg
Préparation
l’échantillon
Preparingde
the
sample
Mini-crushing
10 mm
Mini-broyage
Quartering
Quartage
10 mm
2 ,5 2,5kg
kg
Reduction Quartage
Réduction
2 grilles 2 grids
Quartering
500 g
500 g
Samples
Echantillons
of 500
500g g
de
Sintering and Trempage et
micronisation Micronisation
0 , 5 mm
0,5 mm
Elastomer phase Phase élastomère
Cleaning
Nettoyage
textile fibers
fibres textiles
Séparation
magnétique
Textil
Phasephase
textile
Phase métal
Magnetic
separation
Metal phase
Samples of
Echantillons
de 11 g
Prisespecimen
d’essai
Test
Rotary
Diviseur
dividing table rotatif
Manual
manuelle
Diviseur
rotatif
Rotary
dividing table
Samples
ofde00,7,
,7 ,1,1et& 2 mg
Echantillons
2 mg
Using used tyres as sources of fuel – reference values and characterisation protocols
© Copyright Aliapur – R&D – July 2009
Page 13 of 26
2. Detailed protocol – the constraints and requirements for each
stage
a) Sampling procedure to obtain a sample that is representative of a
batch of ELT
The sample can be taken either on the shredding site or at the level of the storage site of the
product in transit (during loading or unloading). In the case of samples taken on the shredding
site, the samples will be representative of one to several days’ production (depending on the
duration of the sample – or 25 to 250 tonnes of products). In the case of samples taken during
loading or unloading at the storage site, the samples will be representative of several weeks’
production (between 1,500 and 2,500 tonnes of product). The batch samples thus vary
between 15 kg and 200 kg.
The sample taking procedure must respect the main requirements listed below:
→ The sample must be taken at the jetty, using a tool of the open, rectangular shovel
type
→ The shovel is manipulated, for example, by a loader, respecting a detailed procedure
that is adapted to the site’s conditions
→ The increment taken is considered to be valid if for 25 kg of increment taken the result
is at least 20 tonnes
For the test programmes composed of analyses, each increment or set of increments is
considered to be site samples and must be reduced to samples for laboratories and/or tests,
of a maximum weight of 25 kg.
b) Preparing the sample
There are no references on this subject. Given the particular characteristics (particularly cut
resistance) attributed to tyres, Aliapur has sought and developed a strict operating procedure.
The procedure makes it possible to reduce by up to 0.5 mm (with a view to determining the
parameters of the chemical composition type) one or several increments making up the site
sample, if necessary after the determinations of the dimension type, which are non
destructive.
Reference studies:
→ Preparation and analysis of 7 batches of primary shredding of ELT – LRCCP on behalf
of Aliapur, November 2007
→ Complementary analyses of 4 batches of primary shredding of ELT – LRCCP on
behalf of Aliapur, April 2008
→ Sampling and characterisation of aggregates of ELT – BRGM on behalf of Aliapur,
July 2006
The preparation of the sample consists of a reduction made in several stages of
fragmentation/quartering until the different subpopulations present (elastomer, metal wire,
textiles) are obtained. The standard means and procedures for reducing site samples are
carried out in a laboratory with the appropriate equipment.
The operating procedure for preparing the sample makes it possible to obtain 3 distinct
phases, the presentation of which makes it possible to carry out representative analyses
(homogenous material). It must be strictly respected so as to know the precise distribution of
each phase and be able, ultimately, to establish the chemical composition of the sample.
Weigh-ins are carried out at each stage of the sample reduction process.
Using used tyres as sources of fuel – reference values and characterisation protocols
© Copyright Aliapur – R&D – July 2009
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The main stages for reducing shredded tyre samples are as follows11:
1. Mini-shredding: size reduction in a chipper unit (shredder of a typical capacity of 200
kg/h), successively using at least three different grills so as to attain a level of 10 mm
2. Quartering of the 10 mm sample so as to obtain a sample of 2.5 kg
3. Reduction further of the size with the same chipper unit with at least two different
grills
4. Quartering so as to obtain 4 samples (corresponding typically to 500 g of rubber).
Quartering makes it possible to thus limit the total quantity of ELT to be shredded more
finely in view of the following micronisation stage (reduction of the initial sample to a
sample of roughly 2.5 kg).
At the end of these reduction / quartering stages, the metal phase is separated magnetically
and then sorted manually by type of family of metal wire (in relation to their size and shape).
The textile phase is obtained after all the aspiration phases. The textile fibres are then
cleaned. The two phases obtained in this way are immediately ready for the test sampling.
5. Magnetic separation of the metal subpopulation (mainly metal phase)
6. Cleaning the textile fibres recovered at various levels (mainly textile fibres)
Moreover, the study carried out at the request of Aliapur by the BRGM on the aggregate from
used tyres (comparable to the mainly rubber part of shredded tyres) made it possible to
quantify the heterogeneity of the composition of the material, the origin of one of the
components of the sampling error, and to determine the degree of precision engendered by
the sampling from a given mass. It was thus highlighted that the correct sampling of 500 g
from this phase, the size of which is less than or equal to 8 mm, makes possible good
representivity of the sample with regard to its particle size distribution.
A micronisation of the mainly rubber phase is needed to eliminate the problems
associated with the heterogeneity of the make-up of the material. Thus micronisation at 500
µm of an aggregate of 4 mm results in sufficient homogeneisation of the material with regard
to Cu and Si contents (corresponding to the two most variable elements in the sample).
7. Sintering of the powdered sample (mainly rubber phase) in liquid nitrogen and then
micronisation of the powdered sample up to 0.5 mm (ultra-centrifugal shredders
with a 12-toothed rotor)
c) Test sample
The test sample for the mainly textile phase is carried out manually, guaranteeing that the
sampling zone is visually representative of the textile phase.
With regard to the mainly rubber phase, the powder obtained by micronisation is divided by a
rotary dividing table, following the quantities required for the determinations that have to be
carried out.
With regard to the mainly metal phase, the different populations of metal wire can be sent
directly for analysis.
8. Storage and dispatch of the samples obtained for the required determinations
9. Writing a report on the above process, including the weights determined at the
various stages.
11
See Appendix D for information on the procedure for reducing a sample from a shredding site into a sample for tests or a
sample for laboratories in the project for the standard XP 47-EPT dated 17 November 2008
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C. The analysis methods specific to used tyres
The average composition for shredded ELT has been defined as follows:
→ Carbon (C), hydrogen (H), oxygen (O) and nitrogen (N) content
→ Sulphur (S), chlorine (Cl), fluorine (F) and bromine (Br) content
→ Content in 10 major elements (Ca, Cu, Fe, K, Mg, Na, P, Si, Ti and Zn)
→ Content in 16 minor elements (Al, As, Ba, Be, Cd, Co, Cr, Hg, Mo, Mn, Ni, Pb, Sb, Se,
Tl and V)
Analysis methods recommended for determining the elementary composition of a
sample of shredded ELT:
During preparation of a sample of shredded ELT for analysis, different phases are recovered
in the course of the successive shreddings after aspiration, sieving and magnetisation:
A mainly elastomer
(rubber) phase
Phase 1
A mainly metal phase
A mainly textile fibre phase
Phase 2
Phase 3
For each of the phases, adapted analysis methods have been validated. The elementary
composition of the sample is calculated on the basis of the analysis results of each phase,
with weighting in relation to the mass report calculated during the preparation of the shredded
ELT sample.
The following tables present the methods recommended for each phase and for the following
parameters:
→ Humidity of the samples
→ NCV
→ Carbon content
→ Sulphur content
The methods used for the other parameters are specified in the Appendix.
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Mainly rubber and textile (1 and 3) phases: methods respecting
European standards
Mass of
Elements
General principle
the test
analysed
sample
the projects for
Uncertainties
regarding the
measurements
Humidity
The sample was dried at 105°C, in nitrogen or
in a vacuum, until there was a constant weight
per 60 minute period. The humidity content (in
%) was calculated from the loss of mass of the
sample.
prCET/TS 15414-3
1g
NCV
Analysis using a bomb calorimeter of the
increase in temperature following combustion
prCEN/TS 15400
0.3 g
Complete oxidation of the sample at 1000°C in
oxygen. Analysis of the combustion gases after
in
a
reduction
furnace
Carbon (C) passage
(chromatographic column, thermal conductivity
content
detector (TCD))
prCEN/TS 154 07
1 mg
from ± 0.1% to
± 0.2%
Combustion in a bomb containing pressurised
oxygen. Dissolution in an absorption solution
Sulphur (S) (water or a solution of KOH), then analysis
content
carried out with chromatography
prCEN/TS 154 08 and EN ISO 10304
500 mg
from ± 4% to
± 11%
Mass of
the test
sample
Uncertainties
regarding the
measurements
Mainly metal (phase 2) phase:
Elements
analysed
Humidity
General principle
Idem phases 1 and 3
1g
The sample underwent combustion in a flow of
pure oxygen in an induction furnace at 1,600°C.
The carbon was transformed into CO2 and
carried by the oxygen flow to the infrared
Carbon (C) detector.
content
ISO 15350: Steel and iron – Determination of
total carbon and sulphur content – Infrared
absorption method after combustion in an
induction furnace
0.5 g
from ± 0.1% to
± 0.2%
The sample underwent combustion in a flow of
pure oxygen in an induction furnace at 1,600°C.
The sulphur is transformed into SO2 and carried
Sulphur (S) by the oxygen flow to the infrared detector.
content
Standard ISO 15350 – Steel and iron –
Determination of total carbon and sulphur
content – Infrared absorption method after
combustion in an induction furnace
0.5 g
from ± 4% to
± 11%
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D. The particular case of analysing the biomass fraction of tyres
Tyres are in great part composed of elastomers, some of which come from natural rubber
(polyisoprene) obtained from the cultivation of rubber. Part of the carbon content of tyres thus
comes from the biomass, and the emissions associated with the combustion of this biomass
fraction are thus considered to be neutral with regards to the greenhouse effect (CO2 of
biomass origin does not contribute to the greenhouse effect, in accordance with the
recommendations of the IPCC and as currently reflected in the EU ETS directive 2003/87/EC,
see annex IV).
Several methods have been explored by Aliapur for determining the biomass fraction of tyres.
The first approach envisaged by Aliapur was to evaluate how much natural rubber there was
in the tyres and thus dose the total concentration in elastomers and then the concentration in
natural elastomers. To do this, the pyrolysis-GC-FID method (standard NF ISO 7270-2) used
initially involves making up a calibration curve by pyrolysing the samples with known
styrene/butadiene/isoprene ratios: samples of known composition were thus analysed by
chromatography for their content in each component so as to make up the calibration curve.
In the second stage, the sample of unknown composition was pyrolysed and analysed by
chromatography under the same conditions and its composition was determined from the
calibration curve.
We nevertheless observed several problems during the application of this method.
→ extraction time before pyrolysis and pyrolysis temperature could disturb the results
→ the presence of brominated butyl could also disturb the results
→ determining the styrene/butadiene/isoprene ratio gives relative values, obtained from
an estimate made on the basis of nomogram abacus and not measured values
→ natural isoprene cannot in any way be distinguished from synthetic isoprene.
In addition, the presence in the tyre of textile fibres of the rayon type and of stearic acid are
also sources of biomass and are not evaluated in this case.
→ Given these limitations, trying to assess the biomass fraction by determining the
concentration in natural rubber using this standard cannot be considered to be a
reliable method.
Aliapur thus preferred another approach, directly analysing the carbon concentration of
biomass origin (by disregarding the molecule from which the carbon biomass originated), that
is, the ASTM D6866-08 method – method B focusing on the biomass carbon12 assay, for this
reason considered to be more accurate.
Whilst waiting for finalisation of the method to determine the biomass, which will be
standardised at the European level, Aliapur has chosen to use the ASTM D6866-08 method
that is recognised in the United States, and has determined the % of carbon biomass at the
level of the 12 samples taken in 2007 and 2008 by the BETA laboratory, ISO 17025 certified.
This method has in addition been standardised by Aliapur on model mixtures (of known
composition).
→ Aliapur thus recommends using the ASTM method for measuring the carbon14,
adapted to all phases (elastomer and textile).
12
Determining by mass spectrometry the C14/C12 ratio producing the “modern carbon” fraction in relation to the “fossil carbon”
fraction. Fossil carbon does not contain radioactive carbon as its age is considerably greater than the half-life (5,730 years) of
C14.
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III.Appendices
Appendix I: Bibliographical sources
→ Préparation et analyse de 7 lots de broyats primaires de PUNR – LRCCP pour le
compte d’ALIAPUR – novembre 2007
→ Analyses complémentaires de 4 lots de broyats primaires de PUNR – LRCCP pour le
compte d’ALIAPUR – avril 2008
→ Echantillonnage et caractérisation de granulats de PUNR – BRGM pour le compte
d’ALIAPUR – juillet 2006
→ ASTM D6866-2008 Standard Test Methods for Determining Biobased Content of
Solid, Liquid and Gaseous Samples Using Radiocarbon Analysis
→ Projet XP T47-756 du 31 janvier 2008 – norme expérimentale publiée par AFNOR sur
l’échantillonnage et le prélèvement de produits issus de broyage primaire
→ Service R&D d’Aliapur 2008 – Caractérisation de broyats de pneus usagés –
Composition Elémentaire
→ STRATENE – Etude sur les broyats de PUNR en fours Cimentiers – 17 octobre 2006
→ Les combustibles utilisés par l’industrie cimentière – Rapport provisoire BRGM/RP –
septembre 2008
→ Résultats d’analyses de la teneur en carbone biomasse réalisées sur 12 échantillons
par le laboratoire BETA accredité ISO 17025
Appendix II: Excerpt from the circular dated 01 July 2008 from the
MEEDDAT – dispensation granted for evaluating the biomass
fraction of tyres
Excerpt from the circular dated 01 July 2008 – General dispensation awarded for determining
the biomass fraction of used tyres.
The circular specifies that the method to be considered for taking into account this biomass
fraction of ELT when calculating CO2 emissions and the value of the emission factors
(t CO2/T ELT) is:
Emissions CO2 non-biomass ELT = Qty total ELT * EF total ELT * [1-0.146*(EF biomass ELT / EF total ELT)]
Qty total ELT = total mass of tyres (t)
EF total ELT = global emission factor for the tyres (t CO2/t total ELT)
0.146 = mass fraction for natural rubber
EF biomass ELT = emission factor for natural rubber (t CO2/T rubber)
Or
Emissions CO2 non-biomass ELT = Qty total ELT * 2.21 * [1-0.146*(3.23 / 2.21)]
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Appendix III: Detailed analysis methods for the different phases
Mainly rubber phase: Methods in respect of projected European standards
Elements
analysed
Carbon (C),
hydrogen (H)
and nitrogen
(N) content
General principle
Complete oxidation of the sample at
1,000°C in oxygen. Analysis of the
combustion gases after being in a
reduction
furnace
(chromatographic
column, thermal conductivity detector
(TCD)).
Mass of Uncertainties
the test regarding the
sample measurements
1 to
from 0.1% to
2 mg
± 0.2%
0.7 mg
± 0.1%
prCEN/TS 15407
Oxygen (O)
Pyrolysis of the sample at 1,050°C in a
nitrogen flow, then on a lining of
amorphous coal at 1,120°C, then on a
garniture of copper oxide at 550°C and
assay of the CO2 formed in an electrolysis
cell.
(SGS method)
Sulphur (S),
chlorine (Cl),
fluorine (F) and
bromine (Br)
content
Content in 10
major elements
(Ca, Cu, Fe, K,
Mg, Na, P, Si,
Ti and Zn)
Combustion in a bomb containing
pressurised oxygen. Dissolution in an
absorption solution (water or a solution of
KOH), then analysis carried out with
chromatography
1 mg
prCEN/TS 154 08 and EN ISO 10304
Digestion method (mineralisation and
solubilisation of the mineraliser) without
nitric acid: microwave digestion with a
mixture of hydrofluoric and hydrochloric
acids, then assay of the elements by
means of inductive coupling plasma –
mass spectrometry (ICP-MS).
500 mg
prCEN/TS 15410 and NF EN 13656
Content in 16
minor elements
(Al, As, Ba, Be,
Cd, Co, Cr, Hg,
Mo, Mn, Ni, Pb,
Sb, Se, Tl and
V)
Digestion method (mineralisation and
solubilisation of the mineraliser) without
nitric acid: microwave digestion with a
mixture of hydrofluoric and hydrochloric
acids, then assay of the elements by
means of inductive coupling plasma –
mass spectrometry (ICP-MS).
prCEN/TS 15410 and NF EN 13656
from ± 4% to
± 11%
from ± 5% to
± 23%
300 to
from ± 5% to
500 mg
± 22%
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In relation to the standard projects, it should be noted that given the nature of ELT, aluminium
was considered to be a minor element and zinc a major element.
Phase based mainly on textile fibres: Methods in respect of projected European standards
Elements
analysed
Carbon (C),
hydrogen (H)
and nitrogen (N)
content
General principle
Complete oxidation of the sample at
1,000°C in oxygen. Analysis of the
combustion gases after being in a
reduction
furnace
(chromatographic
column, thermal conductivity detector
(TCD)).
Mass of
the test
sample
Uncertainties
regarding the
measurements
1 to
from 0.1% to
2 mg
± 0.2%
0.7 mg
± 0.1%
prCEN/TS 15407
Oxygen (O)
Pyrolysis of the sample at 1,050°C in a
nitrogen flow, then on a lining of
amorphous carbon at 1,120°C, then on a
lining of copper oxide at 550°C and assay
of the CO2 formed in an electrolysis cell.
(SGS method)
Sulphur (S),
chlorine (Cl),
fluorine (F) and
bromine (Br)
content
Content in 10
major elements
(Ca, Cu, Fe, K,
Mg, Na, P, Si, Ti
and Zn)
Combustion in a bomb containing
pressurised oxygen. Dissolution in an
absorption solution (water or a solution of
KOH), then analysis carried out with
chromatography
500 mg
from ± 4% to
± 11%
prCEN/TS 154 08 and EN ISO 10304
Digestion method (mineralisation and
solubilisation of the mineraliser) without
nitric acid: microwave digestion with a
mixture of hydrofluoric and hydrochloric
acids, then assay of the elements by
means of inductive coupling plasma –
mass spectrometry (ICP-MS).
500 mg
from ± 5% to
± 23%
prCEN/TS 15410 and NF EN 13656
Content in 16
minor elements
(Al, As, Ba, Be,
Cd, Co, Cr, Hg,
Mo, Mn, Ni, Pb,
Sb, Se, Tl and
V)
Digestion method (mineralisation and
solubilisation of the mineraliser) without
nitric acid: microwave digestion with a
mixture of hydrofluoric and hydrochloric
acids, then assay of the elements by
means of inductive coupling plasma –
mass spectrometry (ICP-MS).
300 to
500 mg
from ± 5% to ±
22%
prCEN/Ts 15410 and NF EN 13656
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Mainly metal phase:
Elements
analysed
Carbon (C)
content
Hydrogen (H)
content
Nitrogen (N)
content
General principle
The sample undergoes combustion in a flow
of pure oxygen in an induction furnace at
1,600°C. The carbon is transformed into CO2
and is carried by the oxygen current to the
infrared detector.
Mass of
the test
sample
Uncertainties
regarding the
measurements
0.5 g
ISO 15350: Steel and iron – Determination of
total carbon and sulphur content – Infrared
absorption method after combustion in an
induction furnace
There is no standard at present. This is the
internal laboratory procedure. Method using
thermal conductivity after fusion in an inert
gas flow. The sample undergoes reductive
fusion in a pure nitrogen flow in an induction
furnace at 1,800°C. These conditions lead to
the decomposition of the hydrogenated
compounds present in the alloy and induce
hydrogen degassing. The hydrogen is carried
by the nitrogen flow until the thermal
conductibility detector.
The sample undergoes reductive fusion in a
pure helium flow in an induction furnace at
1,800°C. These conditions lead to the
decomposition of the nitrogenated compounds
present in the alloy and induce nitrogen
degassing. The nitrogen is carried by the
helium flow to the thermal conductibility
detector.
0.5 g
0.5 g
ISO 10720: Steel and iron. Nitrogen assay.
Method using thermal conductibility after
fusion in an inert gas flow
Oxygen (O)
content
The sample undergoes reductive fusion in a
pure helium flow in an induction furnace at
1,800°C. These conditions lead to the
decomposition of the oxygenated compounds
present in the alloy and induce oxygen
degassing. The oxygen is carried by the
helium flow to the infrared detector.
0.5 g
NF EN 10276-2: Chemical analysis of ferrous
materials – Determination of the oxygen
content of steel and iron – Part 2: infrared
method after fusion under inert gas
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Element
analysed
Sulphur (S)
content
General principle
The sample undergoes combustion in a pure
oxygen flow in an induction furnace at
1,600°C. The sulphur is transformed into
SO2 and is carried by the oxygen flow to the
infrared detector.
Mass
of the
test
sample
Uncertainties
regarding the
measurements
0.5 g
ISO 15350: Steel and iron - Determination of
total carbon and sulphur content – Infrared
absorption method after combustion in an
induction furnace
Chlorine (Cl)
content
Fluorine (F)
content
There is no standard at present. This is the
internal laboratory procedure. The sample is
mineralised in a nitric acid solution and then
the chlorine contained in the solution is
dosed by means of potentiometry.
0.5 g
There is currently no standard
Bromine (Br)
content
The sample is mineralised in a royal water
solution (mixture of 2/3 hydrochloric acid and
1/3 nitric acid), and the mineral elements are
quantified by induced coupling plasma atomic
emission spectrometry (ICP-AES).
Content in 10
major elements
(Ca, Cu, Fe, K,
Mg, Na, P, Si,
Ti and Zn)
1g
ISO 10278 – Steel. Determination of
manganese content. Inductively coupled
plasma atomic emission spectrometric
method
ISO 13898: Steel and iron – Determination of
nickel, copper and cobalt contents –
Inductively coupled plasma atomic emission
spectrometric method
ISO 13899: Steel – Determination of Mo, Nb
and W contents in alloyed steel. Inductively
coupled
plasma
atomic
emission
spectrometric method
ISO/TR 17055: Steel – determination of
silicon content - inductively coupled plasma
atomic emission spectrometric method
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Elements
analysed
General principle
Mass of
the test
sample
Uncertainties
regarding the
measurements
The sample is mineralised in a royal water
solution (mixture of 2/3 hydrochloric acid
and 1/3 nitric acid), and the mineral
elements are quantified by atomic emission
spectrometry with induced plasma (ICPAES).
Content in 16
minor elements
(Al, As, Ba, Be,
Cd, Co, Cr, Hg,
Mo, Mn, Ni, Pb,
Sb, Se, Tl and
V)
ISO 10278 – Steel. Determination of
manganese content. Inductively coupled
plasma atomic emission spectrometric
method
ISO 13898: Steel and iron – Determination
of nickel, copper and cobalt contents –
Inductively
coupled
plasma
atomic
emission spectrometric method
ISO 13899: Steel – Determination of Mo,
Nb and W contents in alloyed steel.
Inductively
coupled
plasma
atomic
emission spectrometric method
ISO/TR 17055: Steel – determination of
silicon content - inductively coupled plasma
atomic emission spectrometric method
1g
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Appendix IV: Results of analyses methods on the elementary
composition of Passenger car and Truck ELT
Trace elements (< 0.06%)
Passenger cars
Trucks
Aluminium (Al)
0.04 to 0.05 %
0.01 to 0.02 %
Arsenic (As)
0.0001 to 0.0007 % 0.0004 to 0.0005 %
Barium (Ba)
0.001 to 0.002 %
0.001 to 0.005 %
Bromine (Br)
0.02 to 0.03 %
0.04 to 0.06 %
Chlorine (Cl)
0.02 to 0.03 %
0.01 to 0.04 %
Chromium (Cr)
0.002 %
0.003 to 0.004 %
Cobalt (Co)
0.01 %
0.02 to 0.03 %
Copper (Cu)
0.02 %
0.02 to 0.04 %
Magnesium (Mg)
0.02 to 0.03 %
0.02 to 0.04 %
Molybdenum (Mb)
0.0002 to 0.0008 % 0.0002 to 0.0003 %
Nickel (Ni)
0.002 %
0.002 to 0.003 %
Phosphorus (P)
0.01 %
0.01 to 0.02 %
Lead (Pb)
0.001 to 0.002 %
0.001 to 0.003 %
Potassium (K)
0.03 to 0.03 %
0.02 to 0.03 %
Sodium (Na)
0.03 to 0.06 %
0.01 to 0.02 %
Titanium (Ti)
0.006 to 0.01 %
0.004 to 0.005 %
Trace elements (< 0.001 %), for which certain values are at the Quantification Limit
QL at 0.0009 %: Selenium (Se)
QL at 0.0007 %: Antimony (Sb), Beryllium (Be), Vanadium (V)
QL at 0.0003 %: Mercury (Hg)
Trace elements (< 0.002 %), for which certain values are at the Quantification Limit
QL at 0.002 %: Fluorine (F)
QL at 0.0003 %: Cadmium (Cd), Thallium (Tl)
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Appendix V: Detailed analysis results for 10 batches of shredded used tyres
Characterisations of 12 reference batches sampled and analysed in 2007 and 2008
SHREDDED ELT of the Passenger Car type
Global mass balance
Large
A_SGS_076560_EUREC
Large
A_SGS_076557_GRANUL
ATEX
Small_A_Rorichmoor from
Ecoval
Medium A_Antora from
Norvalo
Medium A_Ewald from
Caux Broyage
Large A Gilles Henry – VL2
Large A Trigone – VL3
Large
A
Eurec
Environnement – VL5
Average Reference
Values
Min
Max
Sampling conditions
Combustible characteristics
NCV
Rubber
MetalTextile BIOMASS
%S
%C
MJ/kg
80.90
12.16 6.93
17%
29.9
1.39 68.5
18 kg taken by SGS for 5
production days (250 tonnes)
April-08
24 kg taken by SGS for 2
production weeks (250 tonnes)
June-08
82.54
10.05 7.41
18.9%
30.6
1.43
70.1
138 kg taken by SGS during
loading of a 2,306 tonne barge
August-07
82.30
13.15 4.55
17.0%
29.9
1.29
68.2
160 kg taken by SGS during
loading of a 2,500 tonne barge
November07
80.30
13.57 6.13
18.4%
29.5
1.34
67.5
55.4 kg taken by SGS during
loading of a 1,550 tonne barge
December07
83.59
10.77 5.64
20.3%
30.6
1.36
69.9
May-07
83.08
84.54
84.03
11.25 5.68
12.58 2.89
12.28 3.68
18.1%
17.3%
19.4%
30.4
30.3
30.3
1.36
1.24
1.27
69.5
69.0
69.1
25.6 kg taken from the shredder
outlet during production of 50
tonnes
June-07
82.7
12.0
5.4
18.3%
30.2
1.3
69.0
17.4 kg taken from the shredder
outlet during production of 25
tonnes
80.3
84.5
10.1
13.6
2.9
7.4
17.0%
20.3%
29.5
30.6
1.2
1.4
67.5
70.1
22 kg taken from the shredder
outlet during production of 25
tonnes
June-07
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SHREDDED ELT of the Truck type
Global mass balance
Rubber
Large B Trigone – PL0
Sampling conditions
Combustible characteristics
MetalTextile BIOMASS
NCV
MJ/kg
%S
%C
27.8 kg taken from the shredder
outlet during a one-week
production (60 tonnes). The
chemical analysis revealed a
certain “weakness” in this
sample
March-07
29.8 kg taken from the shredder
outlet
during one ½-day
production (20 tonnes). The
chemical analysis revealed a
certain “weakness” in this
sample
May-07
78.74
21.26 0.00
30.7%
28.35
1.11
65.51
Large B Gilles Henry – PL1 79.67
20.33 0.00
31.4%
28.68
1.12
66.29
Large B Trigone – PL4
73.66
25.50 0.84
29.7%
26.71
1.22
62.56
Large B Eurec – PL6
72.55
27.45 0.00
28.6%
26.12
1.60
59.70
Average Reference Values 73.1
26.5
0.42
29.1%
26.4
1.4
61.1
33.4 kg taken from production
of 5 tonnes
June-07
Min
72.5
25.5
0.00
28.6%
26.1
1.2
59.7
119.1 kg taken from production
of 5 tonnes
June-07
Max
73.7
27.5
0.84
29.7%
26.7
1.6
62.6
Comments on the presentation of the results tables
1)
2)
3)
4)
5)
All the samples were prepared by mini-shredding until separation into the three phases, rubber, metal and textile
The weighting between phases was brought up to 100% (excluding losses and waste)
The NCV, sulphur and carbon content, and the biomass % were the result of the weighted average for the NCV, S, C and biomass C for each of the phases
The NCV, C and sulphur in each phase were analysed on VL2, VL3, VL5, PL4 and PL6
The C biomass was analysed in each of the phases for all the samples.
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