Preparation and Characterization of Chitosan - Agar Blends - Rheological and Thermal Studies

8/3/2016 PREPARATIONANDCHARACTERIZATIONOFCHITOSAN/AGARBLENDS:RHEOLOGICALANDTHERMALSTUDIES
JournaloftheChileanChemicalSociety ServiciosPersonalizados
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Articulo
J.Chil.Chem.Soc.v.55n.1Concepcin2010
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http://dx.doi.org/10.4067/S071797072010000100031
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J.Chil.Chem.Soc,55,on1(2010),pg:130136
Referenciasdelartculo

Comocitaresteartculo
PREPARATIONANDCHARACTERIZATIONOF Traduccinautomtica
CHITOSAN/AGARBLENDS:RHEOLOGICALAND Indicadores
THERMALSTUDIES
CitadoporSciELO
Accesos
ESAM.A.ELHEFIAN*1,MOHAMEDMAHMOUDNASEF2,ABDULHAMID Linksrelacionados
YAHAYA1ANDRASHIDATTAKHAN1
Compartir
1DepartmentofChemistry,FacultyofScience,UniversityofMalaya,
Otros
50603KualaLumpur,Malaysia
2ChemicalEngineeringDepartment,FacultyofChemicalandNatural Otros
ResourcesEngineering,UniversitiTeknologiMalaysia,81310UTMSkudai,
Johor,Malaysia Permalink
ABSTRACT
Inthiswork,anumberofmixtureaqueoussolutionsofchitosan/agar(CS/AG)atdifferentratios(considering
chitosanasthemaincomponent)wereprepared.Therheologicalpropertiesi.e.shearingviscosityandshear
stressoftheblendsolutionsasafunctionofshearrateaswellasthethermalpropertiesoftheblendfilms
wereinvestigated.Amongtheparametersstudiedweretemperature,shearingtimeandstoragetime.Results
showedthatalmostNewtonianbehaviorwasobservedattemperaturesfrom40Cto55Cfortheratios100/0,
90/10,80/20and70/30.However,theproportions60/40and50/50showedaclearshearthinningbehavior
(pseudoplasticnonNewtonianbehavior).ItwasalsofoundthatalltheblendsolutionsobeyedtheArrhenius
equation.Inaddition,theeffectofshearingtimeontheshearingviscosityofallblendsdidnotshowany
significantdifferencesatallshearingtimesappliedinthisstudyexcepttheproportion50/50whereindecreasing
inshearingviscosityandshearstresswasobservedastheshearingtimeincreased.Furthermore,different
behaviorswereobservedfortheblendsolutionswhentheperiodofstoragewasextendedtothreeweeks.The
FTIRresultsandthedifferentialscanningcalorimetery(DSC)curvesshowedthattheinteractionbetween
chitosanandagarcanoccur.
INTRODUCTION
Polymericmaterialhasbeenextensivelyusedinourdailylife.Recently,polymerblendshavereceivedmuch
attention.Thisismainlyduetothefactthatnewmaterialswithbetterphysicochemicalpropertiescanbe
observedwhentheindividualcomponentsusedtoblendarecompatible[1,2].Modificationofchitosanby
blendingwithotherpolymericmaterialsmightbeofinterestforsomeapplications.Lotsofchitosanblendsand
compositeswithotherpolymershavebeenproposedintheliterature,forexample,chitosan/cellulose
membrane[3,4],chitosan/starch[5],chitosan/gelatin[6]andchitosan/collagen[7].Thecompatibilityof
chitosanwiththesepolymersmaybeobtainedsincechitosanisconsideredasastronglyinteractingpolymer
[8].
Chitosan,14linked2amino,2deoxy,Dglucan,isapolycationicderivedfromchitinbyalkaline
deacetylation[9].Duetotheaminogroupsthatchitosanpossessesinitschain,itcanbedissolvedindilute
aqueousacidsolutions,suchasaceticacidandpropionicacid.Sinceitisinexpensive,nontoxicandpossesses
http://www.scielo.cl/scielo.php?script=sci_arttext&pid=S071797072010000100031 1/15
potentiallyreactiveaminofunctionalgroups,chitosanhasbeenevaluatedfornumerousapplications,including
medicine,food,cosmeticsandwastewatertreatment[1014].
Agarisamixtureofpolysaccharideswhichisextractedfromthefamilyofseaweeds(Rhodophycae).Itmainly
consistsofagaroseandagaropectin[15].Theformergovernsthegellingabilityofagar.Thelatterincludes
ionicgroupssuchassulfateandmethoxygroups.Themostimportantpropertyofagarisitsabilitytoform
reversiblegelssimplybycoolinghotaqueoussolutionsduetotheformationofhydrogenbonds[1618].Some
ofitshydrogelblends,suchasPVPagarhydrogel,havealreadybeenprepared[19].Agarhasawidevarietyof
usesinindustry.Forexample,ithasbeenusedinthefoodarea(processedcheese,icecream,breadandsoft
candy)duetoitsabilitytoformhardgelsatverylowconcentration[20,21].
Therheologicalbehaviorofchitosansolutions[2225]aswellitsthermaldecompositionandstability[2629]
havebeenalreadyreportedintheliterature.However,toourknowledge,nomuchworkhasbeendoneon
chitosan/agarblends.Therefore,thepresentworkisaimedatstudyingtherheologicalproperties,i.e,the
effectsofshearrate,temperature,shearingtimeandstoragetimeontheshearingviscositiesandshear
stressesofaqueoussolutionsofchitosan/agarblendsatdifferentproportions.Thisworkisalsoaimedat
studyingthethermalpropertiesofchitosan/agarfilmswiththeviewtofurtherexplorethethinfilmproperties
anditsapplications.
EXPERIMENTAL
MATERIALS
Shrimpsourcechitosanwaspurchasedfromalocalcompanywithadeacetylationpercentage(DD)of88.1%
definedbyUVmethod[30].Thischitosanwasacidsoluble,whitecoloredandflaky.Agarwaspurchasedfrom
Sigma.Aceticacid(glacial100%,proanalysi)waspurchasedfromMerck(Darmstadt,Germany).Ultrapure
water(MximaUltrapureWater,ElgaPrimaCorp,UK)witharesistivitygreaterthan18M2/cmwasusedto
prepareallsolutions.Allchemicalswereusedwithoutfurtherpurificationandfreshlypreparedsolutionswere
usedinallexperiments.
Preparationofthesolutions
Chitosanwasdriedintheovenuntilaconstantweightwasobserved.Then,5gofchitosanwasdissolvedin500
mLaceticacid(0.1M)followedbymildstirringandheatingatabout60Covernighttoform10gL1chitosan
solution.Thesolutionwasthenfilteredtoremovedustandothertracesofimpurities.Airbubbleswere
eliminatedbykeepingthesolutionsatroomtemperaturefor2hours.
Forpreparingagarsolution,thesameamountandprocedureasforchitosanwereappliedwithexceptionof
usingaceticacid,whereinpreheatedUltrapurewaterwasused.Thesolutionswerethenstirredandheatedat
about80Cfor2hours.
Preparationoftheblendsolutions
Blendsolutionswerepreparedbyaddingtheaqueousagarsolutiondropbydroptoachitosansolution,which
waskeptonamagneticstiaring,atabout94C,andthemixturewasstirredatamoderatespeedfor30min.
Thefinalcompositionofchitosan,agar(CS/AG)variedfrom90/10to50/50byvolume.Table1showsthe
designationandcompositionsforallthesolutionspreparedinthisstudy.
Preparationofblendfilms
Thepreparationofblendfilmsofchitosanandagarwascarriedoutatvariousproportions.Theaqueousagar
solutionwasaddeddropbydroptothechitosansolution,undercontinuousstirringat90Cinvarious
proportionsbyvolume.Therangeoftheaddedagartochitosansolutionwasfrom050vol%.Stirringwas
allowedtocontinufor30minutesaftermixing.Filmsoftheresultinghomogeneoussolutionswereobtainedby
castingprescribedamountsofthesolutionontopolystyrenePetridishesfollowedbydryingat60Cfor48h.
Thefilmswerepeeledoffandkeptunderevacuateddesiccatoroverfreshsilicageluntiluse.Allfilmsobtained
weretransparentandfreeofairbubbles.
Similarfilmsfrompurechitosanandpureagarwerepreparedusingthesamecastingprocedureandusedas
references.
Filmthlckness
Thefilmthicknesswasmeasuredwithadigitalmicrometer(Mitutoyo,Japan)withO.OOlmmresolution.Several
thicknessmeasurementsweretakenatvariouspositionsoneachspecimenandtheaveragevaluewastaken.
METHODS
Molecularweightmeasurements
Themolecularweightofchitosanwasabout5.5x105gmol 1determinedat30Cbygelpermeation
chromatography(GPC)equippedwithaWaters1515HPLCPumpandaWaters2414RefractivendexDetector.
ThecolumnusedwasPLaquagelOH30(8um,300x7.5mm)andthesolventusedwas1%aceticacid.The
molecularweightofagarwasabout1.3x104gmol 1determinedat70Cusingthesamemethod.TheGPCwas
calibratedusingpullulansasstandard.
Viscositymeasurements
RheologicalmeasurementswereperformedonaBrookfielddigitalviscometer,modelDVII+Pro,withan
attachedULadapter.Eachofpurechitosanandpureagarsolutionshadaconcentrationof10gL1whiletheir
composition(CS/AG)rangedfrom90/10to50/50byvolume.Theviscositywasdeterminedin20mLofthe
sampleandtheshearingtimewas15seconds.Forthestoragetimemeasurements,solutionswerekeptatroom
temperatureinglassbottlesinadarkplaceuntilanalysis.Eachmeasurementwasrecordedasanaverage
valueoffivereadingswhenaconstantshearratewasapplied.
FTIRmeasurements
FTIRmeasurementsofblendfilms(lOumthick)wereperformedonaPerkinElmer(model2000)spectrometer.
Thespectrawereobtainedatafrequencyrangeof4000400cm1witharesolutionof4cm1and8times
scanningrate.
DSCmeasurements
DSCstudieswereperformedusingaDSCMettlerToledo(modelDSC822e).Thesampleswerescannedundera
nitrogenatmosphereataconstantrateof10C/min.
RESULTSANDDISCUSSION
Theeffectsoftemperatureontheshearviscosityofchitosan/agarblendsolutions.
Inthisstudy,thesearingratedependentviscosityofCS/AGmixturesolutionsasafunctionofshearrateata
temperaturerangeof40Cto55Cispresentedinfigures1(ag).Highertemperatureswerenotappliedinorder
toavoidthermaldegradationofthepolymersandsolventevaporationwhilelowertemperaturescouldnotbe
appliedduetothegelformationforsomemixtures.Similartothatofmanypolymersolutions,thebehaviorof
theviscositytemperatureinterrelationshipforthesemixturesshowadecreaseofviscositywithanincreaseof
temperature.Ontheotherhand,theNewtonianbehaviorisobservedatalltemperaturesfortheratios100/0,
90/10,80/20and70/30.However,theincreaseinshearingviscosityandtheappearaneeofshearthinning
behaviorareclearlynoticedfortheratios60/40and50/50.Itisexpectedthattheincreaseinviscosityfor
CS/AGblendsisattributedtotheformationofhydrogenbondingduetotheinteractionamongthefunctional
groupsofchitosanandagar(OHandNH2groupsinchitosanandOHgroupsinagar).
Figures17alsoshowtheeffectoftemperatureontheshearstressofchitosan/agarmixturesasafunctionof
shearrate.Shearstressincreasedwithincreasingshearrateforallratios.Atthesameshearrate,shear
stresseswerehigheratlowertemperatures.Inaddition,increasesinshearstresswithincreasingshearrate
weremoreremarkableatlowertemperatures.Fromthegraphitisclearthatonlytheproportions60/40and
50/50exhibitpseudoplasticnonNewtonianbehavior.Theresultsofpurechitosansolutionobtainedshowsome
goodagreementwithpreviousstudies[31].Inaddition,thesefiguresindcatethatthetemperaturehasmore
effectonthesolutionsatlowershearratevalues,i.e.,theviscosityincreaseassociatedwithtemperatureis
lessimportantathighshearrates.Thisbehaviorwasalsoreportedintheliteratureforchitosansolutions[32].
Therelationshipbetweenshearviscosity(determinedataconstantshearrate)andtemperatureforCS/AG
blendsandthepurecomponentsisdemonstratedinfigure2.Thisgraphshowsanearlylinearrelationship
(Table1)wherebyviscosityofthemixturesolutionsdecreaseswithincreasingtemperature,i.e.,itisastrong
functionoftemperature.Itcanalsobenotedthatthemosteffectedsolutionbytemperatureisthepureagar
solutionfollowedbytheratioof50/50.
Theviscosityvaluesobtainedataconstantshearratecanbecorrelatedwithtemperatureaccordingtothe
Arrheniusequation:
whereAisaconstantrelatedtomolecularmotion,Ea istheactivationenergyforviscousflowataconstant
shearrate,RisthegasconstantandTistheabsolutetemperatureinK.Aplotoflnviscosityasafunctionof
l/TshouldproduceastraightlineandfromitsslopetheEncanbecalculated.Figure3presentsanArrhenius
plotforvariousproportionsofCS/AGmixturesolutions.Thisgraphalsoshowslinearrelationships.Thevalues
oftheapparentactivationenergyareshownintable2.
Thevalueoftheactivationenergyofchitosanisinaccordancewiththereportedvalues.Forexample,Wangand
Xu(1994)[33]reportedthattheactivationenergyvaresfrom25kJmol 1whenDDis91%to15kJmol 1
whenDDis75%forachitosanconcentrationof20gL1(in0.2MAcOH/0.1MAcONa).Desbrieres(2002)[31]
reportedvaluesofactivationenergyatzeroshearratevaryfromabout15kJmol 1to37kJmol 1fora
chitosanconcentrationrangebetween0gL1and40gL1respectively(solvent,0.3MAcOH/0.05MAcONa).
TheeffectsofshearingandstoragetimeontheapparentviscosityofCS/AGsolutions.
Viscositymeasurementswereperformedasafunctionofshearratefor15.30,45,60and75secondsat40C
tostudytheshearingtimeeffectasshowninfigure4(af)(itwasdifficulttostudytheeffectofshearingtime
forpureagarduetoitsrandombehavioratthistemperature).Atallshearingtimes,CS/AGblendsolutions
exhibitsimilarbehaviorandnosignificantchangewasobservedwithexceptionoftheratio50/50wherein
increasinginshearingtimeleadedtodecreasinginsharingviscosityandshearstress.Inaddition,different
behaviorswereobservedfortheblendsolutionswhentheperiodofstoragewasextendedtothreeweeksata
constantshearrate(Figure5).purechitosanshowedgradualincreaseinviscositywhileadropinviscosityfrom
about130cPto35cPwasrecordedwithinthefirstweekforpureagar,afterwhichitdecreasedgradually.
However,allCS/AGblendsolutionsrecordedabigincreaseinviscositywithinthefirstandsecondweekswhile
adifferenttrendwasobservedinthethirdweek.Therapidincreaseinviscositywithtimemayindcatethat
somestronginteractionshavetakenplaceamongthechainsofthetwopolymers.
FTIRanalysis
Thespectraofpurechitosanfilmandpureagarfilmarepresentedinfigure6.Thespectrumofpurechitosan
filmshowsabroadbandat3367cm'whichisduetotheOHstretching.Thebandat1560cm1isassignedfor
theNHbending(amideII)(NH2)whilethesmallpeakat1647cm1isattributedtotheC=0stretching(amideI)
0=CNHR.Thebandsat2927,2884,1411,1321and1260cm1areassignedtoCH2bendingduetopyranose
ring.Thebandat1380cm1isduetoCH3wagging.Thecharacteristicfeaturesofchitosanspectruminthis
studyaresimilartopreviousreports[3436].FTIRspectrumofagarfilmshowsanabsorptionbandatabout
3400cm1whichisassociatedwithOHstretching[37]whilethepeakat2900cm1isattributedtomethoxyl
groups[38].Thebandataround1640cm1isduetothestretchingoftheconjugatedpeptidebondformedby
amine(NH)andacetone(CO)groups[39].Thepeakat1370cm1isassignedtoestersulfate[38]andthe
bandsat1070and930cm1areassociatedwiththe3,6anhydrogalactosebridges[40].
TheFTIRspectraofchitosanandagarblendfilmscontainingvariousagarproportionsarealsoshowninfigure
6.AsummaryofcharacteristicbandsofchitosanandagarblendfilmsispresentedinTable3.Ascanbeseen,
theincreaseintheagarcontentintheblendfilmscausedadecreaseintheintensityofthebandarisingfrom
theNHbending(amideII)at1560cm1ofchitosan.Thiswascoupledwithasimilardecreaseintheabsorbance
bandat1411cm1andanincreaseofbandabsorbanceat1380cm1.Furthermore,thespectraofblendfilms
showthedisappearanceoftheintensivebandat1033cm1thatwasobviouslyobservedinthepurechitosan
filmandchitosan/agarblendcontainingagarcontentof10%.Thisisduetothefactthatwhentwoormore
polymersaremixed,changesincharacteristicpeaksoccurasareflectionofthephysicalandchemical
interactions[41,42].Theseobservationsindcatetheexistenceofgoodmiscibilitybetweenchitosanandagar
thatismostlikelycausedbytheformationofintermolecularhydrogenbondsbetweentheaminoandhydroxyl
groupsinchitosanandthehydroxylgroupsinagar.
Thermalproperties
Figure7showstheDSCfirstruncurvesofpurechitosanfilm,pureagarfilmandtheirblendedfilms.After
drying,allsampleswerekeptinadesiccatorbeforeanalysis.Allcompositionsexhibitedabroadendothermic
peakatadifferentpositionrangingfromabout75Cto84C(Table4).Similarendothermicpeakshavebeen
reportedintheliteratureforchitosanfilm.Forexample,Limaetal[43]andWangetal[44]reportedan
endothermicpeakofchitosanfilmat60.75Cand83Cforfullydeacetylatedchitosanand85%DDrespectively.
Asforpureagar,EldridgeandFerry[45]demonstratedthatagarfilmexhibitsanendothermicpeakataround
90CwhileLyonsetal[46]foundthattheagarfilmshowsanendothermicpeakat110Cwhichishigherthan
theusualreportedvalue.Also,Suzukietal[47]reportedendothermicpeaksofthreekindsofagargelat
differentpositionsrangingfrom75Cto90CAccordingtosomeauthors,thisendothermicpeakisrelatedtothe
meltingtemperature[48].However,itisoftentermedasdehydrationtemperature(TD),attributedtothe
evaporationofwaterassociatedwiththehydrophilicgroupsofthepolymers[49,50]andrefleetsthestrengthof
waterpolymerinteraction[51,52].Thissuggeststhatsomeboundwaterwasstillnotremovedfromthe
sampleswhendriedinthedesiccator.Theseendothermicpeakswereabsentinthesecondruncurve(notshown
here)whichconfirmedthatthispeakisattributedtothewatercontentinthesample.Acloserexaminationof
Figure7revealsthatthereisadifferenceintheendothermicpeakareaforthemembranes,i.e.,theyvaryin
theirwaterholdingcapacity,showingthattheblendedfilmshavehigherwatercontentingeneralthanthepure
components.Thiscouldbeduetotheformationofnewhydrophiliccenters[53].Anotherpointtobenotedis
thatallratioshavecisevaluesofTDtothevaluesofthepurepolymersexceptfortheratio60/40whichshows
ahighervalue.Theshiofthepeakpositiontoahighertemperatureindicatesastrongerinteractionwith
water.Itisbelievedthatthisvariationonthepositionandpeakareaisduetothephysicalandmolecular
changescausedbyblending.Theseresultssuggestthattheinteractionbetweenchitosanandagarmayoccurto
formfilmswithmorestability.
Withrespecttotheglasstransitiontemperature(Tg)ofchitosan,variousvalueshavebeenreportedinthe
literaturerangingfrom23Ctoabout220C[48,52,5457](Table5).ThevariationsonthevaluesoftheTgof
chitosanisprobablyduetothedifficultyinidentifyingitsincechitosanissemicrystalline[58]aswellasdueto
thelargeamountofintraandintermolecularhydrogenbondsinitschain[59].Inaddition,beinganatural
polysaccharide,thesourceandthemethodofpreparationofchitosancaninfluenceitsTg[53].Inthiswork,the
Tgofchitosancouldnotbedetected.
CONCLUSION
ThisstudyhasshownthatthepseudoplasticnonNewtonianbehaviorwasobservedonlyfortheratios60/40and
50/50ofchitosan/agarblendsattherangeoftemperaturestudied.Inaddition,therelationshipbetweenthe
shearingviscosityandthetemperaturecouldbedescribedwiththeArrheniusequation.Thisstudyhasalso
shownthatcurvesoftheapparentviscosityofpurechitosan,pureagarandtheirblendedsolutionsexhibited
similarbehavioratallshearingtimesof1575s.However,theratio50/50exhibitedadecreaseinviscosityand
shearstresswithincreasingshearrate.Furthermore,differentbehaviorswereobservedfortheblendsolutions
whentheperiodofstoragewasextendedtothreeweeks,butanincreaseinviscosityforallblendswithinthe
firstandsecondweekswasobserved.Therapidincreaseinviscositywithtimemayindcatethatsomestrong
interactionshavetakenplaceamongthechainsofthetwopolymers.Theinteractionbetweenchitosanandagar
wasconfirmedbyFTIRandDSC.
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(Received:July21,2009Accepted:January6,2010)
*email:eelhefian@yahoo.com
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Preparation and Characterization of Chitosan - Agar Blends - Rheological and Thermal Studies

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Preparation and Characterization of Chitosan - Agar Blends - Rheological and Thermal Studies

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