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Waste Management 27 (2007) 367374

Pilot installation for the thermo-chemical characterisation

of solid wastes
C. Marculescu , G. Antonini b, A. Badea a, T. Apostol a

U. POLITEHNICA Bucuresti, Spl. Independentei, 313, Bucuresti, Romania
U. de Technologie de Compiegne, BP 20529 60205 Compiegne cedex, France

Accepted 28 February 2006

Available online 17 April 2006


The increasing production and the large variety of wastes require operators of thermal treatment units to continuously adapt the
installations or the functioning parameters to the dierent physical and chemical properties of the wastes. Usually, the treated waste
is encountered in the form of heterogeneous mixtures. The classical tests such as thermogravimetry and calorimetric bomb operate com-
ponent by component, separately. In addition to this, they can analyse only small quantities of waste at a time (a few grams). These
common tests are necessary but insucient in the global waste analysis in the view further thermal treatment.
This paper presents an experimental installation, which was designed and built at the CNRS Science Division, Department of Indus-
trial Methods, Compiegne University of Technology, France. It allows the determination of waste thermal and chemical properties by
means of thermal treatment. Also, it is capable of continuously analysing signicant quantities of waste (up to 50 kg/h) as compared to
the classical tests and it can work under various conditions:

 oxidant or reductive atmosphere (on choice);

 variable temperature between 400 and 1000 C;
 independently set residence time of treated sample in the installation and ow conditions.

The installation reproduces the process conditions from incinerators or pyrolysis reactors. It also provides complete information on
the kinetics of the waste thermal degradation and on the pollutant emissions. Using dierent mixtures of components present in the
municipal solid waste and also in the reconstituted MSW samples, we dened a series of criteria for characterising waste behaviour dur-
ing the stages of the main treatment process such as: feeding, devolatilisation/oxidation, advancement, solid residue evacuation, and pol-
lutants emission.
2006 Elsevier Ltd. All rights reserved.

1. Introduction density, as well as in physical and chemical characteristics.

That is why there is a high number of treatment methods
The concept of using waste as a renewable source of for that waste, each one with its own particularities. In
energy has become a priority in the eld of wastes treat- order to maximize treatment eciency, it is necessary to
ment. The goal of this research consists not only in waste choose the appropriate method for the given waste. Waste
destruction but also in increased recovery of thermal thermal treatment units encounter operational problems
energy from the processes. due to waste variety. Selecting the optimal treatment
There are numerous and various sources of waste; there- method requires the deep knowledge of many physical
fore the resulting waste is heterogeneous in form and in chemical characteristics of the waste to be treated (Tillman,
1991). The only existing tests for characteristic diagnosis
Corresponding author. Tel.: +40 745 133 713; fax: +40 21 411 31 61. are designated for solid wastes, especially coal. These vali-
E-mail address: (C. Marculescu). dated tests, and we refer mainly to thermogravimetry,

0956-053X/$ - see front matter 2006 Elsevier Ltd. All rights reserved.
368 C. Marculescu et al. / Waste Management 27 (2007) 367374

require a high degree of sample preparation, because the waste components. Not all the components are suitable
quantity of analysed substance must not exceed a few for sampling at the dimensions required by these tests,
grams and a micronic granularity. It is dicult to obtain and, furthermore, the components are not always known.
a representative sample for the waste to be analysed, due TGA and the LHV data are necessary but sucient to
to the low quantity required by the test and to the large qualify a product for further thermal treatment (Tillman,
number of components in the sample. Furthermore, con- 1991). Therefore, thermal treatment units have strict oper-
cerning the texture of the waste, it is almost impossible to ational specications and limitations related to: product
achieve micron granularity. Applying these tests on wastes, feeding and advancing systems, ignition delay and minimal
even reconstituted ones, generates more or less accurate residence time, solid residue mechanical behaviour at the
results, even less clear in the case of waste with a poorly unit evacuation section, and combustible reduction rate
dened composition. eciency. These characteristics were not taken into
These are some of the reasons leading to the necessity of account by previous studies probably because they are spe-
developing of other tests that will provide the same accu- cic to industrial installations, but as the aim of each
rate results on the physicalchemical data, analysing research in this eld is the industrial scale application
increased waste samples (measured in kilograms) with a improvement, they should not be neglected.
granularity in centimetres that do not require laborious For a proper analysis of the nature of the solid waste
preliminary preparation. that ts the requirements of thermal treatment installations
At this moment there are no tests that provide global for their elimination, we dened a certain number of fea-
accurate information on the thermal degradation charac- tures to be quantied by an oxidant or non-oxidant (pyro-
teristics of a waste. The most common tests used for the lytic) test. From now on, in this paper they will be called
waste characterisation are the thermogravimetric analysis criteria.
(TGA) and the calorimetric bomb experiment. The rst
one provides data on the mass reduction rate of the sample 2. The experimental device
under oxidant or pyrolytic condition. The mass variation
speed can be converted in degradation kinetics as a func- 2.1. Installation description
tion of temperature and liberated volatiles content (Coz-
zani et al., 1995b). The second test provides data only on The pilot installation used throughout this study was
the low heating value (LHV) of the sample. The content developed in the laboratory of CNRS Science Division,
of volatile substances is an essential piece of information Department of Industrial Methods, Compiegne University
both for oxidant and non-oxidant waste thermal treatment, of Technology, France. It was designed to quantify hydro-
because the end of the liberation phase for these substances dynamics and heat exchanges in a vibro-uidized bed ther-
marks either the beginning of xed carbon oxidation phase mal unit. Fig. 1 presents the simplied scheme of the
in incineration, or the end of the pyrolysis process (Cozzani device. It consists of a tubular rectilinear reactor heated
et al., 1995a; Fontana et al., 1997). Several studies having by circulation of hot ue-gases (natural gas burner) within
as subject the TGA applied to dierent products (Wu an external double envelope. The solid continuously
et al., 1993; Bockhorn et al., 1999) indicated that it is di- advances by vibro-uidized transport. This type of trans-
cult to compare experimental data from dierent studies portation corresponds to a piston-like ow. For instance,
because no standardized way to perform TGA experiments if we consider a transversal section in the solid advancing
exists and because the obtained weight loss characteristics bed, the particle distribution and number in the bed will
strongly depend on the measurement conditions (Raveen- be same all along the transport tube, with no sliding layers.
dran et al., 1996; Varhegyi et al., 1997; Orfao et al., 1999; The speed of advancing solids is set by the installation
Stengsen et al., 1999). In order to determine the shares of vibratory parameters (Socha and Kolze, 1992; Caudron,
single components in an unknown waste mixture, the 1999).
markers of individual components are correlated with the Each solid particle within the tubular reactor undergoes
one of the mixture. This is why the weighed sum method thermal treatment for the same duration. The tube is
(WSM) presented by Cozzani et al. (1995b) is applied. 160 mm in inner diameter and 4000 mm long. Heat
According to the WSM, the devolatilisation behaviour of required by the process is supplied by the circulation of
a mixture can be expressed as the sum of its corresponding hot gases counter-owing the circulation of solids in the
single constituents. The work of Heikkinen et al. (2004) on 3300 mm active zone.
the sensitivity of the calculated mixture composition using The ow rate (up to 50 kg/h) is determined by the feed-
WSM when changing the position and height of the TGA ing ratio and the advancement speed of the product in the
peak of a single component revealed that modifying the installation, and it imposes dierent lling levels of the
peak height has a strong impact on the calculated compo- tube. The feeding system consists of an Archimedes screw,
sition. On the other hand, the LHV (low heat value) data of whose rotation is controlled by a frequency variator.
a waste to be treated gives information only on the waste From the feeding system, the ground waste is pushed
combustion capacity, and nothing more. Nevertheless, forward by screw rotation and dropped into the vibrating
these tests are applicable to clearly dened and sampled transport tube. There it advances in a piston-like move-
C. Marculescu et al. / Waste Management 27 (2007) 367374 369

Natural gas Process gases analysis

Alimentation with towards burner
divided solid and treatment

Heated case

Transport tube

Treatment gas inlet

(comburant or inert) Solid residue
gases analysis

Fig. 1. Functional scheme of the pilot for solid divided waste characterisation.

ment, which is generated by the vertical vibration of the because the particles have to advance on a higher slope
tube; it goes through the heated zone, towards the tube and the phenomenon of rear sliding in the transport tube
outlet, into a cyclone separator. The resulting sub-prod- increases (Neddreman and Harding, 1990).
ucts, gases and solids, are collected using a cyclone that The feed ow inuences only the bed height and the par-
performs the separation of solid residue from gases, so that ticle agitation degree. The residence time variations due to
they can be analysed separately. The residue is collected at the feed ow are negligible. On the other hand, a higher
the base of the separator in an ash/coke collector. After l- feed ow rate will diminish particle agitation due to the
tration and fast cooling in a quench (to avoid dioxin for- increase of the bed height (Akiyama and Yamaboshi,
mation), both process and heating gases are evacuated by 1992).
an exhauster on separate ways. A pressure-control device The hydrodynamic characteristics of the pilot installa-
inside the cyclone separator maintains a constant pressure tion had previously been studied (Porquet, 1994). The main
level inside the tubular reactor. Keeping a constant gas features of the divided hydrodynamic behaviour of the
layer over the solid bed in the tubular reactor allows not divided solid are:
only the control of the thermal treatment atmosphere (oxi-
dant or pyrolytic conditions) but also the evacuation of the  For a xed frequency and eccentricity (impulse) imposed
vapour and gases resulting from the solid treatment pro- by the engines, the residence time becomes longer if the
cess. The device operates at temperatures in the range of tube inclination angle increases.
4001100 C.  For a xed inclination angle and a constant frequency
The adjustable installation parameters for transport the residence time becomes shorter if the load eccentric-
control of the divided solids inside the tube are the follow- ity degree increases.
ing: tube vibration frequency, impulse, tube inclination and  For a xed inclination angle and a certain impulse, the
feed ow rate (Akiyama and Yamaboshi, 1992). residence time becomes shorter if the frequency
In stationary regime, frequency increase involves ampli- increases.
tude decrease (hence solid particle agitation diminishes)
and a shorter residence time for the treated waste. The
installation operates above resonance frequency. Tests 2.2. The samples
proved that an operation frequency below the resonance
point is insucient for initiating the movement of the Our study is based on thermal treatment by vibro-uid-
product. ized transport applied to divided solids. The concept of the
The impulse is imposed by the load eccentricity of the divided solid is, therefore, very important. No mechanical
two electrical engines that power the installation. It is com- device forces the solid waste to advance. Consequently,
mensurate with the eccentricity degree of the loads only the acceleration forces generate particle movement,
attached to the engine shafts, which generate vibration of causing the advancement of the product in the tubular
the engines. As the engines are xed on each side at the reactor. If the solid is not entirely divided (mud-like paste
middle length of the tube, their vibration is transmitted consistency, cotton-like brous consistency), the movement
to the tubular reactor. The more the impulse increases, forces will be more or less compensated by the particle
the shorter the residence time. cohesion forces in an arbitrary and non-quantiable way
The tube inclination refers to the angle between the tubu- (Jaraiz et al., 1992). Therefore, the piston-like ow condi-
lar reactor and the horizontal plan. The residence time of a tions will no longer be achieved. The installation is suitable
particle in the reactor increases with the tube inclination for solids that are easily broken down to granules, with no
370 C. Marculescu et al. / Waste Management 27 (2007) 367374

sticky or textile bre aspect. Tests showed that a fraction purpose of this test is to highlight the problems encoun-
up to 20% of textiles is acceptable in a mixture with other tered during the incinerator alimentation with solid waste.
solid products. Considering the transporting tube diameter Some types of waste to be treated (plastics) change the
(U = 160 mm), the tolerated solid granularity may reach up aggregation phase or structure during the feeding proce-
to 40 mm. Furthermore, the treated sample must have a dure when the temperature increases from the one in the
certain mass balance of granularity: at least 90% of its environment to the one inside the incinerator. Therefore
quantity must have a granularity superior to 1 mm. If this its mechanical characteristics change completely, impeding
condition is not accomplished, the product will start to the product advancement. If the product covers the critical
compact at the feeding inlet, as a result of the vibrating distance inside the heated tube (about 350 mm) until it
forces, like powder (Jaraiz et al., 1992). reaches the treatment temperature without agglomerations,
the SHM criterion is considered positive. Otherwise the
2.3. Limitations product composition is considered inappropriate for the
treatment parameters and has to be modied or the treat-
The technical limitations of this installation are related ment type has to be changed. These data can be grouped
to product characteristics. Some of them require high air in a ternary diagram as an equilateral triangle. The main
ows (enough oxygen for a complete oxidation reaction) classes of components found in a heterogeneous mixture
that can generate ing particles, as a consequence of the of solid waste are placed in the corners (inert, melting
increased air speed through the constant tube section and non-melting combustible fractions). Each mixture is
(ash, solid residue or even particles that did not undergo represented by tokens placed on this triangle. The dierent
the combustion process). Others have an important fusible zones that result separate the compositions into favourably
fraction in the mixture that can melt, generating a soldering or inappropriate maneuverable at elevated temperatures.
process. For the solids with a high percentage of combusti- The tests were performed on a mixture whose composition
ble compounds, the required air for complete combustion is given in mass percentage fractions: PET (granules of
is very important, and, therefore, the gas ow speed above 2.5 mm medium diameter), pine bark (dried and grinded
the solid waste bed in the tube can sensibly increase. The to medium size less than 10 mm) and clay balls (5 mm).
mixture components with a low specic weight start to Fig. 2 presents the SHM diagram for dierent mixtures
move with the gas ow, and, consequently, the homoge- of the above components. It highlights the transition zones
nous aspect of the treated sample begins to alter. There will corresponding to mixtures that meet the requirements of
also be particles that will not undergo the same treatment the previously dened criterion.
period. The only solution is to reduce the air ow rate in The LVF criterion (liberated volatiles fraction) refers to
order to decrease gas speed. The simplest method is to the volatile components in the gaseous substances that
decrease the feed ow rate at the installation inlet or to are generated along the process. It is an intrinsic character-
mix the waste with a certain inert solid fraction in order istic of the solid, or the mixture, regarding its combustibil-
to decrease the LHV of the sample, so that the required ity because under oxidant conditions the rst substances to
air quantity for complete oxidation will diminish. The inert ignite are the volatiles. We conducted devolatilisation tests
solid fraction solution also ts the second main limitation on PET, wood, paper, forge coal and mixtures at tempera-
introduced by the products containing a high fusible frac- tures within the range of 400900 C in an inert atmosphere
tion. In this case the melted components will stick to the created by constant nitrogen ow inside the transport tube.
inert ones and will continue to move.

3. Analyses PET

We established a certain number of criteria for a min-

75% PET
utely detailed characterization of the incineration capacity
of divided solid waste. They allow the identication of solid 25% pine bark
waste behaviour between feeding and evacuation. That is 25% argyle
40% PET
very important from the standpoint of choosing the most 20% argyle
appropriate type of incineration installation. The inuence 50% argyle 40% pine bark
of global functioning parameters (humidity, temperature, 25% PET 50% pine bark
residence time, etc.) has also been studied. The tests have
been carried out both under pyrolytic and oxidant Transition zone 75% pine bark
75% argyle
ARGYLE Negative MAC criterion BARK
3.1. Reductive atmosphere
Positive MAC criterion
The SHM criterion (sample heat maneuverability) refers
to the sample maneuverability at high temperatures. The Fig. 2. MAC criterion ternary diagram for mixtures of wood/plastic/inert.
C. Marculescu et al. / Waste Management 27 (2007) 367374 371

The measured volatile fraction of the mixtures was com- The CFR criterion (combustible fraction reduction) repre-
pared with the calculated one using the weighed sum sents the percentage of the combustible fraction of the
method (WSM) presented by Cozzani et al. (1995b) and product that is consumed by incineration. For a xed res-
volatile fraction of each component from the scientic idence time and operation temperature, only a part of the
the literature. The errors were about 12% caused by inher- combustible fraction of the waste is oxidized. This share
ent experimental limitations. depends on waste composition. Therefore, this parameter
The AFI criterion (agglutination and friability index) is important for the characterization of waste combustibil-
describes the friable and agglutinant features of the solid ity intrinsic properties and is presented in the second part
residue at the end of the treatment process. The product of this paper.
resulting from the pyrolysis stage of the treatment may The LPC criterion (liberated pollutants content). This cri-
be compact or powder-like, friable or not. For instance, terion concerns the amount of pollutant gases produced by
from a mechanical point of view, a waste whose residues the thermal treatment of one mass unit of waste and the
tend to agglutinate into a very resistant solid will not be concentration of each toxic component in the gases. It
incinerated in a grate type installation (Martin, 2001) enables the researcher to choose the appropriate residual
because it is at risk to stick to the mobile parts. The test gas treatment systems for the analyzed waste sample.
is also applicable to the carbon residue from the pyrolysis These tests had been validated on standard combustibles
reactions. This residue is submitted to a compaction and (wood and coal) under reductive and oxidant atmosphere
friability test, derived from the method in the Roga before being applied to reconstituted waste. We present
(1974), using repeated 1 mm siftings and refusal centrifu- the results of the main criteria applied on dierent products
gation (for about 5 min). The ratio between the sift refu- treated in the installation.
sal weight of the residue and its initial weight gives the
AFI. For example it varies between 0 void compacting 3.3. Mechanical aspects
capacity (anthracite coal) and 100 highly agglutinant
characteristics (forge coal with 95% of its mass retained When generally speaking about waste, we assume it is
after siftings). The results of the test performed on paper, heterogeneous in size, form and specic weight. Therefore,
PET, wood, and mixtures, indicated AFI values of: 11.5 it is important to know if these characteristics have an
for wood, 55 for a mixture of 50% plastic50% wood, inuence on the residence time in the installation for the
75 for a mixture of 50% plastic50% paper, 65 for a mix- same vibrating conditions. We conducted a series of tests
ture reconstituting a dried MSW sample containing plas- to establish the inuence of granularity and heterogeneity
tic 25%wood 20%paper 45%inert 10%. The AFI (specic weight) on residence time.
criterion has to be correlated with the mechanical charac- Fig. 3 presents the variation of the residence time with
teristics of the target treatment unit. Generally speaking, vibration frequency and the granularity of aluminium balls
an AFI coecient below 70 is suitable for common indus- for a xed impulse (the engines loads eccentricity degree of
trial installations. 35%). The average diameters of the aluminium balls ranged
between 1; 2 and 5 mm. The four curves, obtained for dif-
3.2. Oxidant atmosphere ferent vibrating frequencies, are practically horizontal and
prove that residence time does not depend on the treated
The GID (global inammation delay) quanties the time product granularity, but only on the installation operating
interval passing from incinerator feeding to product igni- frequency. We also noticed that the residence time of the
tion. This criterion is essential in characterizing the com- sample in the tubular reactor decreases when the vibrating
bustibility of a certain waste. It shows the capacity of frequency increases. This variation is asymptotic to a
analysed product to ignite, rapidly or slowly, after being certain value, and we assume it is the inferior time limit.
introduced into the incinerator. In the case of our installa-
tion, taking into account the transport type (piston-like
ow), this delay can be estimated considering the position
of the ame front from the device inlet. This position can 90 21 Hz 17 Hz
Residence time [sec]

be determined by measuring the temperature inside the 80 25 Hz 19 Hz

tube with a thermocouple. The tube reactor lengthwise 70

temperature prole has a peak, revealing the ame front 60
existence. The global inammation delay is the ratio 50
between the ame front distance to the transport tube inlet
and the advancing speed of the particle. It strongly depends 20
on the content of volatiles (LVF criterion) and the humid- 10
ity of the product. The test showed that LVF variation 1 1.5 2 2.5 3 3.5 4 4.5 5
from 15% to 90% involves GID decrease from 50 to 10 s. Granularity [mm]
The humidity variation within the 235% range increased Fig. 3. Residence time variation with the vibration frequency for dierent
the GID by about 50%. aluminium balls diameters.
372 C. Marculescu et al. / Waste Management 27 (2007) 367374

Considering the transport tube length (meaning the heated ln1  CFR=100 B  ts 5
zone of the tubular reactor the active zone, about That leads to the conclusion that the logarithmic curve
3300 mm), the residence time can be converted in transport function of the residence time (ts) is a line whose slope is
(advancement) speed. B.
A study on the particle segregation depending on their The experimental curves presented in Fig. 4 allow estab-
specic weight showed the independence of the residence lishing CFR as a function depending on waste advance-
time from the product heterogeneity. The tested product ment in the treatment device, for example, along the
was a mixture of paper pieces and aluminium balls with incineration grate of a Martin installation.
an average diameter of about 2 mm. The measured resi- Marking the experimentally established points, we
dence time was the same using dierent samples of argyle notice two distinctive lines with dierent slopes. The rst
balls, pine bark, PET pieces, and mixtures of them. one corresponds to the volatile emission zone (components
that volatilise at temperatures below 450 C) and its slope
3.4. Thermal aspects BMV represents the variation speed itself. Heikkinen et al.
(2004) showed that MSW components such as plastics
A series of tests allowed us to characterise the combus- (excepting PVC) and cellulose (paper, cardboard, packag-
tibility of reconstituted urban waste with the following ing, wood and organic waste) liberate volatile substances
composition given by Martin (2001): vegetal compounds within the range of 400440 C. This phase duration is
35%; paper, cardboard 29%; plastics 14%; inert (glass) about 280 s depending on the composition of the reconsti-
22%. tuted MSW sample. The other line (slope BCF) corresponds
The operating conditions that we imposed during the to the waste xed carbon oxidation. Knowing the residence
tests mirror actual industrial scale units, with a tempera- time on an incinerator grate, for instance, it is possible to
ture of 1050 C and air excess of 1.2 (20% over the stoichi- establish CFR evolution law under industrial conditions
ometric value). These tests were made in order to establish relying only on the waste advancement status.
waste incineration eciency. Therefore, CFR was mea- The installation also enables the researcher to quantify
sured for four dierent residence times CFR variations with the treatment temperature under oxi-
Xm dant conditions for a certain residence time. Fig. 5 shows
% 1
zCOMB this variation for a 600 s residence time for the same sample
m_ m  m_ 0m of reconstituted municipal solid waste with the above-
X m T ; ts 100  % 2
m_ m
where zSCOMB is the combustible mass fraction of the waste, 0
Xm is the mass conversion rate (reduction) for xed temper- BMV = 0,012 s-1
ature and residence time, T is the xed temperature of the -2

process, ts is the xed residence time, m_ m is the waste mass BCF = 0,003 s-1
feed ow and m_ 0m is the solid residue mass ow at the instal-
lation outlet. -6
As the waste has inert components as well as a combus-
tible fraction, in order to establish the product reaction volatiles emission zone fixed carbon decomposing zone

kinetics, it is important to know the mass reduction rate -10

0 100 200 300 400 500 600
of its combustible fraction but not the global mass reduc-
Residence time [s]
tion rate. For that we have to take into account the
uncombusted (unoxidized) fraction in the slag. Knowing Fig. 4. CFR variation with the residence time for reconstituted urban
the initial inert fraction of the waste, we can calculate the waste.
combustible fraction reduction rate: Xc(T, ts). The two
parameters Xm and Xc are related by the equation:
Xm 93
Xc % with K the waste inert fraction. 3 91
1K 89
CFR [%]

Eq. (4) connects the CFR of collected solid residues to the 87

unoxidized fraction XIMB from the slag:
100 S zSIN 81
CFR S z  X IMB % 4 79
zCOMB COMB 100  X IMB 77
where zSIN
is the inert mass participation in the waste and 450 500 550 600 650 700 750 800 850 900 950

XIMB is the unoxidized fraction in the slag. Temperature [grd C]

The CFR denition can be transposed for a xed tem- Fig. 5. CFR variation with the reactor temperature (residence
perature in: time = 10 min).
C. Marculescu et al. / Waste Management 27 (2007) 367374 373

100 idence time distribution, independent from the solid bed

95 properties. Tests showed the independence of the treated
product residence time (from 4 up to 40 min) from its gran-
CFR [%]

ularity and specic weight if the product components with
less than 1 mm granularity do not exceed a maximum of
80 10% in the mixture. The mass ow ranges from about
75 1 kg/h up to 50 kg/h, depending on the product specic
weight. The treatment atmosphere is adjustable to research
0 20 40 60 80 conditions: from pyrolysis with less than 1% oxygen to
Inert fraction in the mixture [%] combustion with air excess up to 1.51.8. The dened cri-
teria for waste mechanical and thermo-chemical character-
Fig. 6. Inuence of the inert fraction in the sample on the CFR variation
(residence time = 10 min, temperature = 900 C). isation are fully quantiable and appropriate for the
simulation of industrial scale thermal degradation of solid
heterogeneous mixtures.
mentioned composition. This kind of test can be accom-
plished for dierent residence periods within the opera- References
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