1

Dielec ic cha ac e iza ion o biodeg adable was es 1
du ing py olysis 2
D. Bene oso1, A. Albe o-O iz2, J. Monzó-Cab e a2, A. Díaz-Mo cillo2, A. 3
A enillas1, J.A. Menéndez1* 4
1Ins i u o Nacional del Ca bón, CSIC, Apa ado 73, 33080 O iedo, Spain 5
2Depa men o Communica ion and In o ma ion Technologies, Technical 6
Uni e si y o Ca agena, Ca agena, Spain 7
Co esponding au ho : Tel.: +34 985 119090 8
E-mail add ess: [email p o ec ed] 9
10
Abs ac 11
The lack o dielec ic p ope ies da a has o en been named as one o he 12
easons ha has hampe ed he simula ion o mic owa e p ocessing o 13
biomass eeds ock and p ocess design. In his wo k, he dielec ic beha io 14
o an o ganic ac ion om municipal solid was es du ing py olysis has been 15
moni o ed as a unc ion o empe a u e. Fu he mo e, he e ec o he 16
addi ion o a mic owa e abso ben ma e ial (ca bonaceous cha ) o he aw 17
biowas e upon he dielec ic p ope ies has been in es iga ed o he i s 18
ime. 19
The e iciency o he con e sion o mic owa e ene gy o hea , measu ed by 20
means o he an δ pa ame e , is shown in his s udy o be nea ly 20 imes 21
highe when he abso ben cha is added o he eac ion bulk a oom 22
empe a u e and his gap is e en g ea e in he 600 – 800 ºC ange. 23
Ne e heless, he esul s sugges ha he addi ion o inc easing amoun s o 24
mic owa e abso ben (up o ca. 40%) impai s mic owa e pene a ion, which 25
gi es ise o a less homogeneous hea ing o he bulk. The e is he e o e an 26
op imum p opo ion ha balances hea con e sion and pene a ion dep h. 27
The esul s o his s udy lend suppo o he use o cha as a means o 28
induce he mochemical ea men s by mic owa es and educe ene gy 29
consump ion in he p ocess. 30
31
Keywo ds: Dielec ic p ope ies, Mic owa e py olysis, Biomass py olysis, 32
Mic owa e hea ing modeling, Mic owa e abso ben 33
34
2

1. In oduc ion 1
On a e age, e e y one o he mo e han 500 million people li ing in he 2
Eu opean Union (EU) h ows away a ound hal a on o household ubbish a 3
yea . This is on op o he huge amoun o was e gene a ed om ac i i ies 4
such as manu ac u ing (360 million ons) and cons uc ion (900 million 5
ons), while he supply o wa e and he p oduc ion o use ul ene gy 6
gene a e ano he 95 million ons. Al oge he , he EU p oduces up o 3 7
billion ons o was e e e y yea [1]. A signi ican p opo ion o was e going 8
o land ill is o ganic ma e ial, (i.e. de i ed om bo h biomass and pe oleum 9
sou ces). The mochemical con e sion p ocesses, in ol ing py olysis and 10
gasi ica ion, can con e his was e a sou ce in o po en ially use ul 11
chemical eeds ocks and uels a e he emo al o he mo e eadily 12
ecyclable ma e ials, such as me als, glass, e c. 13
14
A numbe o p ocesses a e now unde de elopmen o a e a he 15
demons a ion s age, whose aim is o p o ide mo e cos -e ec i e, 16
en i onmen ally and socially accep able al e na i es o incine a ion plan s. 17
One o hese new echnologies is mic owa e py olysis based on dielec ic 18
hea ing. This p ocess bene i s om he main ad an ages o using 19
mic owa es, such as apid, olume ic and selec i e hea ing, and a oids he 20
need o sh ed he eeds ock and o p e-d y he samples, esul ing in a 21
subs an ial educ ion in he cos s associa ed wi h hese s eps [2-5]. In spi e 22
o hese ad an ages, his echnology has no ye eached indus ial scale 23
3

owing o he lack o economic analyses on a la ge scale and he absence o 1
su icien da a o quan i y he dielec ic p ope ies o he inpu eeds ocks. 2
3
The p ope y ha de e mines he dielec ic esponse o ma e ial unde he 4
in luence o an elec ic ield is he ela i e complex pe mi i i y, ε*, which is 5
exp essed as a unc ion o a eal componen known as he dielec ic cons an 6
(which ep esen s he abili y o dielec ics o s o e elec ical ene gy) and an 7
imagina y componen known as he dielec ic loss ac o (which ep esen s 8
he abili y o a ma e ial o abso b he elec ic ene gy): 9
10
11
12
whe e and ε’ and ε’’ a e he dielec ic cons an and he dielec ic loss 13
ac o ela i e o he co esponding dielec ic p ope ies o ee space. 14
15
An es ima ion o hese p ope ies is essen ial o he e ec i e design and 16
scaling up o mic owa e hea ing p ocesses o ensu e an accu a e p edic ion 17
o he abso bed powe densi y; i.e. he a e a which he elec omagne ic 18
ene gy is con e ed o hea in he ma e ial. Dielec ic p ope ies may a y 19
wi h composi ion, equency, empe a u e and e en ma e ial densi y [6] 20
and, he e o e, i is essen ial o cha ac e ize hei a ia ion in ela ion o 21
hose pa ame e s. 22
23
4

Se e al s udies ha e a emp ed o cha ac e ize he dielec ic p ope ies o 1
coal [7] and some kinds o biomass [8, 9] since i is known ha he dielec ic 2
loss o hese ma e ials a low empe a u es is negligible, making hem 3
anspa en o mic owa es. Howe e , when he subs a es a e subjec ed o 4
highe empe a u es (i.e. empe a u es highe han 600 ºC), he s uc u es 5
become essen ially cha , which is known o be a high mic owa e abso bing 6
ma e ial due o he Maxwell-Wagne e ec which causes a e y high 7
displacemen o π-elec ons on ca bonized s uc u es [10]. I is o his 8
eason ha di e en mic owa e ecep o ma e ials a e added o biomass 9
du ing mic owa e py olysis, so ha a high enough empe a u e is eached 10
o induce py olysis [11, 12]. Howe e , mos published s udies a e ocused 11
solely on he dependence o dielec ic p ope ies upon equency adia ion a 12
oom empe a u e [13-16] and igno e he need o a comp ehensi e s udy o 13
he whole mic owa e py olysis p ocess. In o he wo ds, an in-dep h and 14
ex ensi e s udy o he dependence o dielec ic p ope ies on empe a u e is 15
needed o ob ain a be e unde s anding o he dielec ic esponse o o ganic 16
subs a es du ing mic owa e py olysis and o mixed o ganic subs a es 17
when used wi h mic owa e suscep o s. 18
This pape in es iga es he mic owa e abso p ion capabili y o a 19
biodeg adable was e and i s mix u e wi h mic owa e abso ben cha on he 20
basis o hei dielec ic p ope ies, om oom empe a u e up o 800 ºC a 21
he commonly used equency o 2.45 GHz. 22
23
2. Ma e ials and Me hods 24
5

2.1 Biowas e p epa a ion and cha ac e iza ion 1
The biodeg adable was e used o his s udy was an o ganic ac ion om a 2
municipal solid was e, ob ained om a land ill in Se ille (Spain). The was e 3
was d ied, pa ially cleaned o ine s such as glass o me als and size-4
educed o 1-3 mm. This ac ion has been labelled as MSWd. The p e-5
ea men o his o ganic esidue allows a good homogenei y o his ac ion. 6
Ac ually, his ac ion has been used in o he s udies o p oduce syn hesis 7
gas by means o mic owa e-induced py olysis and he composi ion o he gas 8
was qui e homogeneous when epea ing he es s [17]. 9
In o de o assess he e ec o adding cha as mic owa e abso be o he 10
biowas e upon he dielec ic esponse, a ca bonaceous solid cha was 11
p epa ed by subjec ing he biowas e sample o a empe a u e o 800 ºC in an 12
elec ic u nace o 1 h in an oxygen- ee a mosphe e. This has been labelled 13
Cha -MSWd. The mix u es o cha :biowas e we e p epa ed in weigh a ios 14
o 0.3:1 and 0.6:1. These wo mix u e a ios we e conside ed on he basis o 15
keeping he amoun o cha as low as possible o induce he mic owa e 16
py olysis. In p e ious s udies [17], we used 0.3:1 a io; hus, we ha e used 17
his same a io in his wo k. Fu he mo e, a la ge amoun (0.6:1 a io) was 18
conside ed o s udy he e ec o adding cha o eeds ock as mic owa e 19
abso ben . 20
The mois u e, ash con en and ola ile ma e da a o he esidues we e 21
ob ained on a LECO TGA-601 de ice. To pe o m he ul ima e analysis, a 22
LECO-CHNS-932 mic o-analyze and a LECO-TF-900 u nace we e used. 23
The mic o-analyze p o ided da a on he ca bon, hyd ogen, ni ogen, and 24

6

sul u pe cen age composi ion. The oxygen con en was de e mined using 1
he LECO-TF-900 u nace. The esul s o p oxima e and ul ima e analyses 2
o he MSWd and cha -de i ed samples a e p esen ed in Table 1. 3
4
Table 1. P oxima e and ul ima e analyses o he MSWd and Cha -MSWd ac ions 5
Residue Municipal
solid was e
Cha om
municipal
solid was e
Label MSWd Cha -MSWd
Mois u e 2.8 3.3
Asha 27.7 66.6
P oxima e
analysis
(w .%) Vola ile
ma e a 61.1 1.7
C 45.1 30.7
H 5.4 0.1
N 2.1 1.0
S 0.4 0.7
Ul ima e
analysis
(w .%)
O 19.3 0.9
6
2.2 Measu emen o dielec ic p ope ies 7
An in e se me hodology o ob ain he pe mi i i y o he di e en biowas es 8
was used (Fig. 1) [18]. This echnique is one o he mos app op ia e; o he 9
echniques such as s anda d coaxial p obes may lead o lowe p ecision 10
since ai bubbles below he coaxial p obe can esul in lowe alues o 11
pe mi i i y; esonan -ca i y echnique is ypically used o low-loss 12
ma e ials (which is no ou case) and iden i ying he esonan equency and 13
quali y ac o (in insic pa ame e s o his echnique) would ha e been 14
di icul due o he high abso p ion o he ma e ials. Fi s , each sample (see 15
Sample R in Fig. 1) was in oduced and uni o mly compac ed in o a qua z 16
ube (i.d. 5 mm, heigh 43 mm; MSWd bulk densi y: 166 kg/m3; cha bulk 17
7

densi y: 353 kg/m3) and hea ed up o a speci ic empe a u e in an oxygen-1
ee a mosphe e by a GALLUR con ec ion o en. The samples we e subjec ed 2
o 25, 50, 100, 200, 300, 400, 500, 600, 700, 800 and 1000 ºC be o e being 3
e y quickly placed (maximum 3 s) in he middle o a WR-340 wa eguide 4
whe e he sca e ing pa ame e s (i.e., S11, S12, S21 and S22) we e measu ed 5
by means o a RHODE & SCHWARZ, model ZVA67 ec o ne wo k analyze 6
se o a equency o 2.45 GHz. S-pa ame e s desc ibe he esponse o an N-7
po ne wo k o ol age signals a each po . The i s numbe in he 8
subsc ip e e s o he esponding po , while he second numbe e e s o 9
he inciden po . Thus S21 means he esponse a po 2 due o a signal a 10
po 1. A e wa ds, he measu emen sys em was modeled (Sample S in Fig. 11
1) by using CST Mic owa e S udio (CST MWS) comme cial so wa e and, by 12
in e se echniques, he alue o he complex pe mi i i y o each sample a 13
he co esponding empe a u e was ob ained. Tha is o say, an op imiza ion 14
me hod (a gene ic algo i hm combined wi h a g adien descen op imiza ion 15
me hod) [18] was applied o he model o ob ain a simula ed ma e ial ha 16
would induce he same sca e ing pa ame e s as hose p e iously measu ed. 17
As ini ial alues o he co esponding op imiza ion me hod, he 18
pe mi i i y o he ma e ials was measu ed in a po able DIMAS 19
dielec ome e , model DIELKITV/DIELKITC a oom empe a u e. The 20
e o s du ing measu emen s a e included in he Supplemen a y Ma e ial. 21
Fu he mo e, o minimize he unce ain y o he sample cooling on he 22
pe mi i i y measu emen s du ing he sample ans e om he o en o he 23
wa eguide, he cooling cu e was p e iously es ima ed and can be ound in 24
8

he Supplemen a y Ma e ial. This cu e allows es ablishing he ope a ing 1
empe a u e o he o en in o de o each he nominal empe a u e in o he 2
wa eguide. 3
4
FIGURE 1 5
6
2.3 Loss angen calcula ion 7
The loss angen is an impo an dielec ic p ope y which is di ec ly ela ed 8
o he abili y o a speci ic ma e ial o con e elec omagne ic ene gy in o 9
hea a a gi en empe a u e and equency. This p ope y is de ined as: 10
11
12
13
Fu he mo e, he ela ionship be ween he dielec ic p ope ies o biowas e 14
and cha was in es iga ed o he wo ma e ial mix u es o e he selec ed 15
empe a u e ange. The dielec ic p ope ies o a mix u e o wo di e en 16
ma e ials can be modeled by using di e en equa ions such as he Landau, 17
Li shi z and Looyenga equa ion (Equa ion 3), as epo ed in [19]: 18
19
20
21
whe e is he olume ic ac ion o he ma e ial MSWd, which was 22
calcula ed om i s densi y, and and a e he pe mi i i y o 23
he biomass and cha ac ions, espec i ely. The accu acy o his model was 24
9

es ed using he expe imen al da a ob ained o e he empe a u e ange 1
selec ed. 2
3
2.4 Skin dep h calcula ion 4
The skin dep h, also known as pene a ion dep h (Ds), is de ined as he 5
dis ance om he su ace in o he ma e ials a which he a elling 6
elec omagne ic wa e powe d ops o e-1 om i s alue a he su ace. The 7
skin dep h can be calcula ed using Equa ion 4 [20]: 8
9
10
11
whe e is he mic owa e wa eleng h in ee space. The skin dep h is an 12
impo an pa ame e since he use o mic owa es as a hea ing medium 13
usually in ol es scaling-up limi a ions due o he di icul y o p ope ly 14
dispe sing he mic owa es as he ma e ial inc eases in olume [21]. 15
16
3. Resul s and Discussion 17
The measu ed dielec ic p ope ies o he MSWd and Cha -MSWd ac ions 18
a e shown in Fig. 2 (a) and (b), espec i ely, e sus he inc ease in 19
empe a u e. As can be seen, he dielec ic p ope ies depend g ea ly on he 20
empe a u e du ing py olysis, pa icula ly a high empe a u es. 21
FIGURE 2 22
The dielec ic cons an and loss ac o o MSWd show a nea ly cons an 23
alue om oom empe a u e up o 500 °C, co esponding o he py olysis 24
16

4. Conclusion 1
The dielec ic p ope ies o an o ganic ac ion om a municipal solid was e 2
we e de e mined a 2.45 GHz om oom empe a u e o 800 ºC. The 3
dielec ic p ope ies o he biowas e emained cons an du ing py olysis up 4
o 400 ºC; hen he e was a sha p inc ease in bo h he dielec ic cons an 5
and loss ac o , owing o he elease o ola iles and honeycomb-like ca bon 6
s uc u es wi h a high delocalised elec on densi y. Fu he mo e, he 7
addi ion o cha as mic owa e abso ben o he eeds ock p o ed o be an 8
e ec i e way o educe he ene gy consump ion o he py olysis p ocess, 9
because i p o ided he bulk wi h a high an δ a oom empe a u e, 10
al hough i educed he pene a ion dep h, which esul ed in a mo e 11
he e ogeneous hea ing when a high concen a ion o cha was used. 12
The dielec ic cha ac e iza ion add essed in his pape could se e as a 13
s a ing poin o he design o sui able equipmen o pe o m he 14
mic owa e-induced py olysis a indus ial scale wi h he app op ia e 15
simula ion so wa e. 16
17
Acknowledgmen s 18
The esea ch leading o hese esul s has ecei ed unding om he 19
Eu opean Union’s Se en h F amewo k P og amme o esea ch, 20
echnological de elopmen and demons a ion unde g an ag eemen n° 21
311815 (SYNPOL p ojec ). D. B. also acknowledges he inancial suppo 22
ecei ed om PCTI and FICYT o he Go e nmen o he P incipado de 23
As u ias. 24

17

Re e ences 1
2
[1]Eu opeanCommission,Beingwisewi hwas e: heEU’sapp oach owas e3
managemen ,in,2010.4
[2]D.Bene oso,J.M.Be múdez,A.A enillas,J.A.Menéndez,In eg a edmic owa e5
d ying,py olysisandgasi ica ion o  alo isa iono o ganicwas es osyngas,Fuel,1326
(2014)20‐26.7
[3]V.L.Buda in,P.S.Shu lewo h,J.R.Dodson,A.J.Hun ,B.Lanigan,R.Ma io ,K.J.8
Milkowski,A.J.Wilson,S.W.B eeden,J.Fan,E.H.K.Sin,J.H.Cla k,Useo g een9
chemical echnologiesinanin eg a edbio e ine y,Ene gy&En i onmen alScience,410
(2011)471‐479.11
[4]F.Mo asemi,M.T.A zal,A e iewon hemic owa e‐assis edpy olysis echnique,12
RenewableandSus ainableEne gyRe iews,28(2013)317‐330.13
[5]D.Bene oso,J.Be múdez,A.A enillas,J.Menéndez,Mic owa ePy olysiso 14
O ganicWas es o Syngas‐De i edBiopolyme sP oduc ion,in:P oduc iono Bio uels15
andChemicalswi hMic owa e,Sp inge ,2015,pp.99‐127.16
[6]J.B.Salsman,Technique o Measu ing heDielec icP ope ieso Mine alsasa17
Func iono Tempe a u eandDensi ya Mic owa eHea ingF equencies,MRSOnline18
P oceedingsLib a y,189(1990)null‐null.19
[7]Z.Peng,J.‐Y.Hwang,B.‐G.Kim,J.Mou is,R.Hu cheon,Mic owa eAbso p ion20
Capabili yo HighVola ileBi uminousCoaldu ingPy olysis,Ene gy&Fuels,26(2012)21
5146‐5151.22
[8]F.Mo asemi,M.T.A zal,A.A.Salema,Mic owa edielec iccha ac e iza iono hay23
du ingpy olysis,Indus ialC opsandP oduc s,61(2014)492‐498.24
[9]F.Mo asemi,M.T.A zal,A.A.Salema,J.Mou is,R.M.Hu cheon,Mic owa e25
dielec iccha ac e iza iono swi chg ass o bioene gyandbio uel,Fuel,124(2014)26
151‐157.27
[10]J.A.Menéndez,A.A enillas,B.Fidalgo,Y.Fe nández,L.Zubiza e a,E.G.Cal o,28
J.M.Be múdez,Mic owa ehea ingp ocessesin ol ingca bonma e ials,Fuel29
P ocessingTechnology,91(2010)1‐8.30
[11]D.Bene oso,J.M.Be múdez,A.A enillas,J.A.Menéndez,Mic owa epy olysiso 31
mic oalgae o highsyngasp oduc ion,Bio esou ceTechnology,144(2013)240‐246.32
[12]D.Bene oso,J.M.Be múdez,A.A enillas,J.A.Menéndez,In luenceo  he33
mic owa eabso ben andmois u econ en on hemic owa epy olysiso ano ganic34
municipalsolidwas e,Jou nalo Analy icalandAppliedPy olysis,105(2014)234‐240.35
[13]A.A.Salema,Y.K.Yeow,K.Ishaque,F.N.Ani,M.T.A zal,A.Hassan,Dielec ic36
p ope iesandmic owa ehea ingo oilpalmbiomassandbiocha ,Indus ialC ops37
andP oduc s,50(2013)366‐374.38
[14]R.Oma ,A.Id is,R.Yunus,K.Khalid,M.I.AidaIsma,Cha ac e iza iono emp y39
ui bunch o mic owa e‐assis edpy olysis,Fuel,90(2011)1536‐1544.40
[15]S.Ramasamy,B.Mogh ade i,Dielec icp ope ieso  ypicalAus alianwood‐41
basedbiomassma e ialsa mic owa e equency,Ene gy&Fuels,24(2010)4534‐42
4548.43
[16]A.A.Salema,M.T.A zal,Nume icalsimula iono hea ingbeha iou inbiomassbed44
andpelle sunde mul imodemic owa esys em,In e na ionalJou nalo The mal45
Sciences,91(2015)12‐24.46
18

[17]D.Bene oso,J.M.Be múdez,A.A enillas,J.A.Menéndez,Compa ing he1
composi iono  hesyn hesis‐gasob ained om hepy olysiso di e en o ganic2
esidues o apo en ialusein hesyn hesiso bioplas ics,Jou nalo Analy icaland3
AppliedPy olysis,111(2015)55‐63.4
[18]M.E.Requena‐Pe ez,A.Albe o‐O iz,J.Monzo‐Cab e a,A.Diaz‐Mo cillo,5
Combineduseo gene icalgo i hmsandg adien descen op miza ionme hods o 6
accu a ein e sepe mi i i ymeasu emen ,Mic owa eTheo yandTechniques,IEEE7
T ansac ionson,54(2006)615‐624.8
[19]D.C.Dube,S udyo Landau‐Li shi z‐Looyenga's o mula o dielec icco ela ion9
be weenpowde andbulk,Jou nalo PhysicsD:AppliedPhysics,3(1970)1648.10
[20]J.P.Robinson,S.W.Kingman,E.H.Les e ,C.Yi,Mic owa e emedia iono 11
hyd oca bon‐con amina edsoils–Scale‐upusingba ch eac o s,Sepa a ionand12
Pu i ica ionTechnology,96(2012)12‐19.13
[21]J.Douce ,J.‐P.La iole e,S.Fa ag,J.Chaouki,Dis ibu edMic owa ePy olysiso 14
Domes icWas e,Was eandBiomassValo iza ion,5(2014)1‐10.15
[22]M.T ipa hi,J.N.Sahu,P.Ganesan,T.K.Dey,E ec o  empe a u eondielec ic16
p ope iesandpene a iondep ho oilpalmshell(OPS)andOPScha syn hesizedby17
mic owa epy olysiso OPS,Fuel,153(2015)257‐266.18
[23]Y.Fe nández,A.A enillas,J.Á.Menéndez,Mic owa eHea ingApplied oPy olysis,19
Ad ancesinInduc ionandMic owa eHea ingo Mine alandO ganicMa e ials,20
S anisławG undas(Ed.),ISBN:978‐953‐307‐522‐8,InTech,InTech,2011.21
[24]J.P.Robinson,C.E.Snape,S.W.Kingman,De elopinghighpowe mic owa e22
p ocessingasane ec i e echnology o  he he mo‐chemicalcon e siono 23
biodeg adablemunicipalwas e,in:TechnologyREsea chandInno a ionFundP ojec 24
Repo ,Uni e si yo No ingham,2010.25
[25]H.H.Sai ,A.A.Salema,Mic owa edielec iccha ac e iza iono SaudiA abianda e26
palmbiomassdu ingpy olysisanda indus ial equencies,Fuel,161(2015)239‐247.27
28
29
30
31
32
33
19

1
Figu e cap ions 2
3
Figu e 1. In e se me hodology o de e mining he dielec ic p ope ies 4
based on he p ocedu e desc ibed in [18] 5
6
20

1
Figu e 2. Dielec ic p ope ies o he (a) MSWd ac ion (b) Cha -MSWd 2
ac ion du ing py olysis. 3
4
5
21

1
Figu e 3. E olu ion o an δ du ing py olysis o he (a) MSWd and (b) 2
Cha -MSWd ac ions. 3
4

22

1
Figu e 4. Dielec ic cons an o he mix u es 2
3
23

1
Figu e 5. Loss ac o o he mix u es 2
3
24

1
Figu e 6. E olu ion o an δ du ing py olysis o he di e en cha /biowas e 2
mix u es. an δ om MSWd ac ion is also depic ed as a means o 3
compa ison 4
5
25

1
Figu e 7. Mic owa e skin dep h o he mix u es o MSWd wi h Cha -2
MSWd du ing py olysis 3
4
32

1
Mix u e Cha :MSWd (0.6:1) 2
0100 200 300 400 500 600 700 800
0
20
40
60
80
100
120
140
Tempe a u e (ºC)
ε
´
ε
´ s Tempe a u e Ma e ial 3
ε
´
ε
´+U
ε
´
ε
´-U
ε
´
3
0100 200 300 400 500 600 700 80
0
0
20
40
60
80
100
120
140
Tempe a u e (ºC)
ε
´´
ε
´´ s Tempe a u e Ma e ial 3
ε
´´
ε
´´+U
ε
´´
ε
´´-U
ε
´´
4

33

0100 200 300 400 500 600 700 800
0.2
0.4
0.6
0.8
1
1.2
1.4
1.6
1.8
2
Tempe a u e (ºC)
anδ
anδ s Tempe a u e Ma e ial 3
anδ
anδ+U anδ
anδ-U anδ
1
34

1
Cha sample 2
3
0100 200 300 400 500 600 700 80
0
0
20
40
60
80
100
120
140
Tempe a u e (ºC)
ε´
ε´ s Tempe a u e Ma e ial 4
ε´
ε´+Uε´
ε´-Uε´
4
0100 200 300 400 500 600 700 80
0
4
5
6
7
8
9
10
11
12
13
Tempe a u e (ºC)
ε´´
ε´´ s Tempe a u e Ma e ial 4
ε´´
ε´´+Uε´´
ε´´-Uε´´
5
35

0100 200 300 400 500 600 700 80
0
0.05
0.1
0.15
0.2
0.25
0.3
0.35
0.4
0.45
Tempe a u e (ºC)
an
δ
an
δ
s Tempe a u e Ma e ial 4
1
2
36

1
Cooling down cu e 2
50 100 150 200 250 300 350 400 450 500
0
200
400
600
800
1000
1200
Time (s)
Tempe a u e (C)
Cooling cu e
In e pola ed. Max descen : 22.47 C/s
Measu ed
3
4
5