TABORATORIO

NACIONAL
DEENCENHARIA
CIVIL

Proceedings
of the
InternationaI
Symposi
um

in culturalheritage
Stoneconsolidation
research
andoractice
Editors
JoséDelgado
Rodrigues
JoáoManuelMimoso

L l s b o n . 6 -M
7 a y2, 0 0 8
Semñárior€aliadonoLNECem Maio2003

@ LABoRATÓR|O
copyrtghr AC V L, . P
NACONALDEENCENI-IAR
CienlfiGe Técnica
de DivulSaeáo
Div¡sáo
av Do BRASIL101. 1700-066L SBOA

E¡itor:LNEC

Reunióes
Colecqáo e nremaconas
Nacionaú

DescriptoK cuLtufathefitaSe / hte¡natonaLcoñ8re$

/ NatufaLrone/ stoneconsolidation
o
Dscritores: Patri.nón coLtural/
PedranatuGl/ ConseNa!áode Pedrade coNrur6o / Co¡8re$oint€ma'onaL
Descripteuu ParimonecuLtural/ PierenatureLLe
/ de
Consolidation la Plereá batn/ congr¿sintehalonaL

cDU 6912,620r97(063X100)
lsBN 97A-97249 2135-a
Evaluationof Cyclododecaneas a temporary
consolidantfor CulturalHeritagemater¡als
ChiaraAnselmi
PhD Chen¡sfry/PastDoc, SMAArt c/o Dip¡i4imento di Chinica, Uniyersít¿'degli Stu.li di
Perugia,Pe¡"ugia,Iralt, chiaruaús@ínwínd.ít
BrendaDoh¿ y
PhD Chenistry/PosfDoc, 5tr4,4,4rt c/o Dípaúimento.li Chimica, Uníwrsit¿ deBli Stu.Jidi
Perusia,Pe¡"usia,Italy, b.bd.daherr'@tdtkzt.con
FedericaPresciütti
PhD Chemisttj,/PostDac, ktifuto CNRdi Scicnzee TecnolagíeMalecalari (ISTM,
Dipatinento di Chinica, Uniyersitáde&liStudí¡li Perugia,Perugíe,Iab),
fe¡ler ica@thch.unips. iI
CostanzaMiliani
PhD Chenisúy /Researcher,Istituto CNRdi ScienzeeTecnologieMole¿olari (ISTM,
Dipartimen¡adi Chinica, Untuersit¿deglí Studi di Perugia,Perugia,Ifaly,
miliani@rhch.un ¡pg.¡t
BrunettoBrunetti
Professor/Chemist¡yPlatessar, Uniyersía degli Studi di Per gia, Petueia, Italy,
bruno@drn.unips.il
AntonioSgamellotti
Professor/Chemistt),Prcfessor, Unirersüá degli Studidi Perugia,Perug¡a,Laly.
sgan@thch.unipg.il

SUMMARY: Cyclododecane,(Ct,Hu), has been investisated Ior furure use in the lield af
consenatbn as a tenporuty consolidanr for fragile nater¡als af art hitraric inpartance in
situatiotls oJ energency ftdnspoú, excayation or handling. Thís contributian has prinarily
established the citeia Ior sobent applicdfíon of white spir¡ts a d cyclohetune \|here
assessnent of subsequent sublímation hds been fa owed util¡zing partable mid,Infrarcd
ReÍectance Spectrascapy. Furthet dnatyses bj Prcfle NMR-MOUSE (Mobile Unílersat
Su¡face Exploret) were use¿ to sdín infomation on the depths of penetratían af the
cyclododecane h dillercnt stone matices as well a: to folow its eyaporaríon fTon within
the nast potous oJsystens.

KEI WORDS: Cycla¡lodecane, temporary cansoliddrían, water repellent, transpotL

porrahI e instrunentatian

INTRODUCTION
Cyclododecane, (CDD) a vol¿rilecyclicalkane(CrrHr,r), hasbeen(seldon)adoptedfor use
in th€ fi€ld of conservationin the last 15 years as a temporary consolialant,sealanta,nd
hydrophobic prol€ctivecoatingfor ftagilematerialsin situations
of transpor,excavation or
handlingÍ11.Literalureshowseveralpotentialusesof cyclodod€cane for situatio¡swhere
 anJ rmp-egnJrion of lrrdre m Icralsur ob'ecr'¿rede':r¿ble drd
.empordqLUn\olid¿r.on
hr,c bee¡ pooo*d ¡rd 'poraJhall) c'red. br rhe'e(Lnnts ol LrJtsrre arLn¡eorog'cal
g a u / e' r e
n " ' . ' ' , ' ¡ " p o r e r, o n o r ¡ ¿ ' l p a r r r i n ¡s' r n a c' $ ' r l -a l ' ) e f " f i m p ' c g n ¡ r e d
" t.eatments peitonneaon mediawirh diflerentdegreesof water
¿".i.g
"q'.""s
"."t..ii* *.¡ i" t"*r¡.s andp¿perandits useon architectur¿l
l.n"ir;'irv stucturesl2-sl This waxv
."riJ .á.. coulábe greatlvexploitert further as rouli¡e in lbis disciplinedue
", "-p*"*" uupou.p..'rui. which permiis it to subhne completelv within an
i" li"
"¡."o*i'ii. removal bv phvsical o¡ chemical operalions or
appropiatetnne t6l elimi¡arinssubsequenr
unnecessary treatmeDt of residues or by-pfoducts
CDD mav be ideally LLlillzed m lhis field ¿si1hasgoo{tñlnl-fonringpropefies'lorvmelting
s ¡ o . ' i r . i r ' o l u b i l n in ¡ d r e r .' o l u b r l i ti)1 o r g d r ' r5c, ¡ l ' r 1 r sa ¡ d l i r r l e" r 1 o
"',,",,'"í or rs ed'rrvre\ersiblelhr' t)diocrúr1 J
ior^rn 71.Yer ron iTponrnr'vi" appricar
'i;;ii.'br;.' rr no'tporar
tut, .¡i oe ,porie¡ ,i 'n"r'* '','. or .¿1 be üi"o'\e'r
h.loseldred f)d-oLJrbons or peLrole'n erh'n' The
-l'f"''*.¡r'*"i,'*."'"'."i.
i. io|med"' eir\er b1 ruoIng v" rle n'olen. rtulerra' or,b)
,urrl filo of c)cloooJc,"ne
r' Lenl lú e\Jpñ'¿re ior' ¿ salJrared Jlrol ul c]croJooecrne rre
atlolirp lheor|rarrc "u
b\ choosnsone urrl d l'igl rrelrirs poinr'
'.i1.'.,i"" .r;¡. blrJer' c¿nbe erarded
¿ppl)'ns ,r In a norrer srdre. keeorru 'be rre¿red o\jccr rn a con,a'ned e':l'
'etrperatu e' ql :T:1",i:
ll har been
Dr;r;.r';q rhe rcareduL ecr Fonr e\po'r're o elerated
ol rhe slbsrrJre r" úhicl- rr-i"¿pplied
r"rn.'"i ¡",'hL filll 'unlb-.' ro hc ropograph¡
lló. uhe¡e.r. c\¡¿c¡err'rrcs rin) vaD deperJ rg on lhe dpll'¿ ron lrethoJ' Lhoier'Lne
D o r o s ro\ f l h e ' J b s r r " l rer d l h e r a r t o l f i l f i o r m a l r o
l)n l l l l ' i c n rh ) d r o p b o bef l l e ( r '
'vrrl a melr or \ol¿rre bildrng tidord o- n solLlrons-urrh lou boilil'
l;-úJ;,"1.""
.o,veir\ ,rhere.por,r¿reou\ L\roofalron ol sol\err produ'<' a lrlrn-ol vcr) lrnc Irgnry
frllr' Irom erdDo arilg \tl\en's 'onsisr ol larJe corr'¡ cosr¿r:
o"cleJ cr\slr''. "lo$l)
ivhichmakethempemeablero waler[5]
and
in a laboratoryselting,theprelhinary melho{tsof solventapplicationfor wlite spüils
ón diveÁestonesof varving porosities have been invesrigated. The fonnalioD
cvclohexane
1o
oi the differingc¡ystallinefrucrlLfe¿ndnet$'orkdensitvthal is nodified in accordance
of the selecled solvenl has been observed with oplical mlcroscopv
rhe rateof evftoration
an¿iompa¡e¿io trnt orthe lnolte¡ CDD. The assessment of rhe subsequenr subhnationm
Spectroscopv bv
** followed ulilizins portablemid lnfrared Refleclance
","1 ""i" Profile NMF \4OUSl l\4obile
.i"',.".i;i"g 'h. m"¿e'o .r¡rariur'l-unher¿nJl\'esb)
ol rne
Uri'e.al sLIf¡ce t\plorerr úere L'ed lo ob'c e rte deprh' ol penelrJ'rul
resurrn! froí eachsolvent in each stonc natrix as well as to lollow its
;;ú;"";."
evaporalion fron1wilhin ¡hemostporous ofsvstems
of
This coDt¡ibutionhas soughtto developand establishoptimumcriterialbr the.use
r t e á t ¡ " ' r ' e u l t u n r r <a o f l h a r i o r r' o r r ¡ r e i " l ' u f J " l ' i ' r o rh
c v co ¿ o ¡ c . " r e
" i r r 'e{rile,.ar.hieclJr¿l bu',drnü'and5cLlptule' lh¿l rn l le rdrc
In ponrlLe! nrnc y parrrrng..
r¡'e ol cnergen,rreqJfe "1 nmedarednJ'afe inlefverrr'on e'pe'r"ll) 'l rfdgrle anoo- rn
a direstaleofconservation

204
EXPERIMENTAL

Reagentsand samplepreparat¡on
Al1 chemicalreagenlsusedwere of analyticalgr¿dewherepossibleand usedas received.
Cyclododecane waspurchased ftom CTSs.r.l.Italy.Whjtespiritwasacquiredfrom PHASE
in producfsutilizedin restoration
s.r.l.Italy, specialized andcyclohexane
liom J.T. B¿ker.
Stone samples obtained from a local manufaclurer,Pemgia, of Canara marble
scmx5cnax2cm werc polishedusing a gmdedsilicon carbidepaper (240 C). The CDD
solulionwaspreparedulilizing l/l w/v in solvent,followedby gentleheatingandaccurate
splayinsovertheeniireavailablesurface.

Methodsof character¡zat¡on
Portable mid-lnfrared Retleclance Spectroscopy
Non inv¿sivein$aredinvestigaiions havebeencalriedouf with a compactportableFT IR
JASCOVIR ar00 qpec'rophoromerer r50x50\5U Lm: J5 kg weighl'.equipped wirhd fiber
optic exlension.lhe opticalbenchis madeof a Midac llluminatorIR radiationsource,a
Michelsoninterferometer, anda liquidnitrogencooledMCT (MercuryCadmiumTelluride)
deleclor.The Remspecmid-in&aredfiber optic probe consistsof a bifurcatedcable
containing19 chalcogenide glassñbers,7 of which car¡y the infraredradiafio¡frorn the
source1()the sample,while the other 12 collectthe radiationreflecledotT the sample'
surface.T}leacquirable specl¡alrangeis 7000-900cri' at a resolutionof4 cm r. The fible
opticprobeis kept perpendicular to the su¡face(0"/0' geon€try)al a dislanceof about"2-4
mm.Theinv€stigated samplearea,asdeteminedbytheprobediameler.is aboul20mm'.
Thetotalreflectivily,R, due10th€ combi¡€ddiftuseandspecularcomponents, is measured
usi¡g the speclJuln&on an aluminiumminor plale for backgroundcotTectioD. The
spectrum intensilywasdefinedas the pseudoabsorbance A' whereA' - log (l/R). Due 10
samplingprobe geometrycollected signals may confain bolh diftuse a¡d specülar
While difTusereflectioncancauseonly slightshiftsin absorplionbandposilion,
reflections.
as compa¡edro transmission speclra,specularditTusioD may caus€derivaiiveor inverled
bandshape(,"¿srsr,,ari
el?effect).
Thedatahavebeentrealedlo a conslant baselineandthe pseudoabsorbance (an averageof
3 pointswith relevánlerors at eachtimely interval)hasbeenfollowedfor characteristic
bandsofCDD film andlhemarbl€matrix.

Profile NMR-MOUSE(Mobile [Jniversal Surface Explorer)

TheProfileNMR MOUSE[1] 12] is a portableNMR sensoreqüippedwith a sinsle-sided
permanent magnelanangement generalinga uniformslaticmagneticfield gradientsuitable
for highresohüion samptep.ofilingup to depthsofabout7 nrm &om objectsplacednearby.
Its size is approximafely100 ' 100 x 80 mn1r.The working frequ€ncyis 11.6MH4
th€reforethe signalis dueto the decayof hydrogennucleus-The NMR signalde¡ivesftom a
thin slicecentered7 nlm abovethe deviceparallelto its surf¿ce,wher€the field st€ngthis
0.411T and the gradientis 20 T/In alongthe depthdirection.The slicevolumeextends
abou!10 x 10m¡rr alongthe lateraldirections, a sizethai is deteminedby thegeomet¡yof

205
theradio ftequencycoil of thesensor,whilethe thickness on
in thedepthdirecliondepends
the setling of the measurementparametelsand canrangefrom I 80 to 2.1 FÍI.
The sensorjs moüntedon a lift, which canbe positionedwifh a precisionof 10 Fm to scan
the profile by shiftingthe sensitivesliceltuoughthe object.Fot eachslice the tansverse
magnetization decayis collectedwith a multj-echoirain.The measuedsignalis r€ducedto
a T2 weightedprorondensilylvithir the sensilivesliceby pafial i¡tegrationof the echo
envelope. The collectionofthesenumbersas¿ fmclion ofdepih formsthe neasuredNMR
depthprofile. T1 weightingcan also be introducedto the measuremenl by varying the
recycledelaybetweensubsequent acquisitions.By default,therecycledelayis chosenlarge
enoughto avoidTl weighling.The profilea¡¡plitudeat eachdepfhwascomputedfrom the
sumoflhe maxina oI ihe firstechoesjDtheacquiredechotair.

Optical m¡croscope
A LeicaDMR OpticalMicroscope equjpped with a Digilal CaneÉ LeicaDC 300 hasbeen
used. lmages have been captu¡€dusing polarizedvisible light to observesuperficial
moryhologychanges on film form¿tionthroughsubhnalion.

AND DISCUSSION
RESULTS
The insolubilityin polarsolventslike warer,elhanol,or acetoneis ofcentralimportance lbr
the application of CDD in the field of resto.¿1ion.It is only rhroughthischaraclerislic thaia
volatilesealingor addingof hydrophobicfealuresas a protectionagainstwateror other
polar solvenlsbecomespossible.knprovenentsin the applicativemethodstartedwith the
selectionof opportunenon polarsolvenls,whichwasbasedpri¡narilyon thet low toxicily
or non loxicity [13]. This choiceilmedialely excludedaronatjoor halogen¿ied solvents
becauseof lheir provenleve1sof toxicily. Alkan€sand ethers,then, due to iheir great
structural ¿fiinity with CDD and, wilh few exceptions,a relalively low loxiciq7, were the
seer:ringly suitablecompoundclass€s to investigate. This proteciionis nol reachedbecause
of the insolubilityof CDD in polar systemsalone.The consolidatiltg and preseFative
propeliesof CDD dependon the nalure of the filrn formed ¡s a dir€cl resultofhow it is
appliedovera surface.Our obseNalions havesuggested that1()avoidwaterpenetration, tbe
ideál fibn shouldbe not needle'likebul rarhersimilarto a glassamoryhousstructureto
ensue compl€1e coverage ofthe surfacewilhoutthe holesth¿tcanbe foundin needlelike
c¡yslalnels.This typeoffihn is producedon sprayingratherthanbrushi¡gandappears most
similar to the nolten CDD, repo¡l€din rec€ntpublicationsconcludingthat in general,
molten cyclododecane providedbe[er proiectionthan so]venl-hsedspplication[]l as
obseFedin figurela-d.
It was obsenedthat a iow boiling poini solventofers rhe bestsuface coverageandsuch
appearsto h¿ppenbecauseof the evaporalionrale, that when too fast does not appearto
leaveenoughtime for crysialgrowth,andhencethebetlerfilm coverage. For thisreasonwe
first tried to employ solventsnam€ly ¡-butyl melhyl elher and pelroleumether wilh boiling
pointsof 50"Cand40 60"C respectively. Both solvenis,ahhoughshowinggoodsohbility,
have demonstraiedto be 1oo volaú1efor our applicativepurposesas the resuhing
sublimationappears lo havebeenaffectedwith its overallincre¿se in thepresence of highly
volatil€ agentsnal. Thus, our attention was tumed 1() higher boiling poiDt ones ln
paíicular,we haveinvesligaled thebehaviorofcyclohexane. thal is knownto be muchless
toxic than its acyclicanaloguez hexa¡econsideredinsieadto be a neurotoxicsolvent.
Cyclohexane's boilingpoinl (81'C) appeared to be ableto conjugatethe easeof application
to ¿ sufficiently fast evaporalion.I¡deed we found the crystalsfomed wilh cycloh€xaneto
be nore squamous like than ¡reedlelike, ensuringbefter surface coveragevisually.
Funhemore, different concentrationsof CDD in cyclohexanehave beenexanined, finding
l/i w/v to be the nore satisfyingratio. Becausethis concentrationrepresenlsan
overs¿tuatedsolution, gentle heating for a few secondsis necessary10 obtain a
homogeneous sohfion.

Figu¡e l¿ d: Opticalmiooscopeiñaeesxl00 mag.a) natml Caran marble,b) CDD brushed

c) CDD moltenandporredon surfaced) CDD spruyedatplicatio¡.
application,

In the effort of conparison, white spirits, a solvent nomally employed in restoration

envirorn¡ents,afthoughdisplaying a greatertoxiciry, was utiliz€d to monitor the different
behaviorof solvents.wlite spirits is a linear and branchedalkanemixture wil¡ a v¿riable
contentof aromatics(19% in our case)with a boiling ra¡ge betw€en150-185"C.It was
observed,by imagesat the optical microscope,that the solventroo canhavea large effect on
the resultingmorphologyofthe c¡ystalsl15l (figure2a-b)ofrhe CDD film whenthe latler
is sprayedin solulion. This is consideredas an effeci of the parureterc in .he gowing
crystal system,such as the crystal bulk, solution buik and the boündarylayer betweenlhe
crystalandsolutionbulk containing the interface[16].Thesolventcanbe assumed 1oreduce
the growih rate of cryslals and has 1obe removedfiom the surfacebefore the crylal face

Throughoutthe trialsof applicationand solventchojce,fiber optic mid-FTIRwas ableto

definetheefiiciencyofthe film, i.e.whelheror not theresultingfilrn coveredtheunderlying
marblematrix sufiiciently,by the presence or absence of characfedstic bandsof both the
CDD and the marble. Fisure 3 displays speclraof a) natural Canara marble where,in the

207
 ',
spectalregionextendingñom 16001o1400cm thev3tundamental siretchingvibmtionof
the COr' ion is obsened.Thisbehaviouris, mainly,the specularcompo¡enl,which causes
major distofions to occur in the spectra,andevid€nt in this caseis the so calledre.ststrdhl¿n
band[17]. Figure3b) showsa spectrrmofpure CDD, wiih numerouschatacteristic bánds
from 950-1500cmr at 966, 1041, 1076, 1162and 1245 cmr mosfly attributedto
asymnetricC-C sl¡etchingmodesofvibration 1181.Spectrumc) showsthe marbletreated
with CDD, indicafingthe completecoverageof the marblematrix. d) insteadshows¿
specfümof maóle treatedwith CDD afteronew€ek,wheretheCDD is nearlyall sublimed
reveali¡s the marbleundemeath.

imagcsx100mag.of CDD aplied after24h in a) cyclohexane,

Fisu.e2á-brOpticalmicroscope

I --*- --tlt t'"^ (

I
€
b
t1\
/ I
J

L
Wavénumb6.(cm)

Figu¡e 3a-d: FTIR reflectdce spectE of a) natunl Camra CDD sta¡da.d. c) CDD
teaiedúarbleandd) sublimcdCDD on márble.
From this. olher lhan lhe chemical nature ol lhe CDD aDd solveDlcompositionsll9l, rhe
film fonnalion a¡d subsequentsublimation of the CDD ca¡ be monjtored through ba¡ds
j,
both charactcristicof tbe CDD, such as the afbre¡¡cnlioDedband at 1245 cn1 and of Lhe
marble subfrate al 1562 cm', hig¡1ighled in figure 3, that play inporraDt roles in
conLrollingthe surfacesl¡uctureof the film which can si'nply defe¡minethe efticie¡cy oflhe
film fomed with eachsolvenl (ilgure 4).
From figure 4a, it is possibte liotn lbe ch¡racte stic peak of CDD to Dote that both the
solutions of CDD/whiie spirils aDd CDD/cyclohexane behave differently on the marble
surfaceuDderroom lenperalure a¡d pressure,where the rate of lbnnalion ofthe CDD film
is relatedto the evaporationoftbe solventwhich is obse¡\,ed1(]slabilizeaftef circa 6 hou¡s.

É $
¡. 1
¡ s

oflnfraredpeakal a)1245cm r andb) 1562cm againr Lime

Flgure4: Plol ofpscudoabsorbance
(hou6)ofmarblebearedrvithCDD/Fhitcspi|its¡¡d CDDhyclohexán€ reqrcctivcly

Following such.tbe monltoring oIlhe CDD/cycbhexa¡e film sublimalionoccurs consta¡tly

afler 72 hours and the peak at 1245 c111'is no loDger obseNed afte¡ 96 hours. The optical
microscope gives an insjghl of this subhnálior lvhere the film is punctured $,ilh holes
creali¡s i¡creasinsly large lslandsolexposed marble (fisure 5a).

FiSn¡e5a b: Opticai¡ric.oscolennagesxl00 mag.ofCDD ¡ptlied alter9ó houNnr a)

cyclohcranc,b) rvhitespnits.

209
Inslead with CDD/white spi¡its the film appea$ constantfor 72 hou¡s, afte¡ which it too
sublimes completely after 144 hours. This filnl asain obse¡vedwith optical microscopy
shows a similar sublimation,wilh the pres€nceof small holes that incr€aseand exposethe
u¡derlying marble (figure sb). Following rhe same time scale for the appearanceof the
cha.acterjsticbánd of narble (figure ab), il can be observedthai this baÍd grows as the
CDD fil¡¡ sublimesleavingthe marblesubsháte exposed. The CDD/cyclohexane beginsto
noticeably exposelhe maaix atur 72 hours, yet is consideredcornpletebeyond 160 hours
when rhe mal¡ix is more €xposed.The CDD/while spirits süblimationis more lapid a[ef 12
hours¿fterwhichthenatrix beconesincreasingly obseNed10144hours.
Profile-NMR-MOUSE can be very usetul in measuringthe thicl¡ess of the CDD layer
which forms on the surfaceofthe stoDe,as well as nr offering indicationsofils penetralion
insidethe sloneandfollowing its disappearance in ñnction of time.
The plofiles of CDD/white spiriis on Carraramarble in tunction of time are repoÍed in
figure 6a. tt is importanr to obse e that the first profile is very different in shapeand in
amplitudewith respectto the others,probably becausethe high boiling poi¡t solventis sli1l
p¡esent in ihe CDD film and this fact can relevantly alTect the NMR measuremenls.
Thereforeit is impossible1oestimatethe startingthicknessofthe layer, but it is evidentthat
after 24 hoursihe solventis completelyevaporatedandthe thicknessis around270 pm. The
subsequentproñles are characterizedby an increasinsly thimer layer becauseúe CDD
startsio sublime;after 144hoursthe CDD visibly disappeanexceptfor a small island which
fal1sin lheneasuredare¿of lcm'.

t j

I 6-
E E

t|oo 500 500 700 300

100 200 300 ro0
t00 0 100 2¡I0 300 ¡O0 500 600 700
depth(!¡m) depth(pm)
Figure6a b:D?thprofiles measu¡ed onCDD layerappliedon Cararundble at differe¡tiimesin a)
whitespirit¡,b) cycloh€xa¡e.Eachprofileis obtainedusi¡gCPMG" sequencein orderto collect
tn¡sversemag¡etiz¿tion decayss'ith an echotlme rE=0.052ms, rR= 0.15 s, and 256 scans
(depthrcsoluflo¡ 40 pn).

The results collected for CDD/cyclohex¿ne are repofed in figure 6b. tt is noliceable that the
low boiling solvent is alreadyevaporatedaffer 6 hours and the lhicknessoflhe CDD l¿yer is
arcund 470 pm. The CDD siarts to sublime and the layer becomes thinner. After 96 hours
the thicknessis around 280 pm, thereforethe layer has nanowed approximately200 pm. In
both casesthe CDD does not seem10 be penetratinginsjde the stone,most likely due to the
Car¡aG marble's characteristic 1ow Dorositv.

210
 coNcLUstoNs
It has been possible to prelininarily study ihe applicajive mefbods of clctododecane in
differ€nl solvenlsso as 1o acquirean emcienr consolidaringfilm for an appropriareamounl
oftime. In order to p¡oducean emergencyprolocol for the applicationofcyclododecaneto
marble su{aces it has bce¡ possibleto slirdy rhe €ffecr ofdifferenr sotveDtson the duratioD
lJ1 the film. From the numerous solvents studied, resutts have b€en given for rhe use of
cyclohexa¡e and common white spirits. These ¡esulrs show that lhc CDD/cyclohexa¡e
soluiion createsa fi1m thaLcaü be observedwirh FTIR and profile-NMR MOUSE unril ar
least 96 hours, wh€¡easthe CDD/while spi¡i1 solufion can be observedup to 140 hours. IL
has also been possible1oobseNe the decrcasingofthe thicknessofrhe layer and the vhuai
eil¿cls ofsublimalion, suggesti¡gthat rhe CDD sublincs, leaving behind i¡creasingly l¡rye
islands of exposed undc.lying marble. It is shown thár rhe characrerisrjcsof the fit¡¡ aie
decisive. l'he thick¡css and duration ofthe fiim and its morphologicalcharacre¡isrics
.rrethe
mosl critical facto¡sfor its effeclive¡ess.
CurcDl researchhas taken these p¡ch¡inary resutts iúo accounl and nume¡ous orh€r
solvents are being lesled for thei¡ du.abiliry of lhe CDD consolidáringfilm formalion.
Prescntstudieson a Droreporous slone (37.5%) comp¿redro thar of marble (t%) indicate
üat the evaporalionrlte doesnol only dependon rhe chemical nature ofthe compoa¡{t bui
also o¡ the sfruclureoflhe impregnatedsyslem.Penet.atinginto ¿ nrore porous syrem
[20]
or r¡to a more degradedsystemappcarsto imply a more prolonged evapomtionmle rhanon
non porous sound systems.Extemál factors aftecting Lherate ofsubhnalion are also being
tale¡ i o conside¡alion.such as varialions in temperalure.humidity a¡d ventilatjon.

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