SiQUADRASORBTM

SURFACE AREA & PORE SIZE ANALYZER

© 2008 Quantachrome Corporation 0608 07160 Rev.CQUAN

TACH

ROME

QUADRASORB™ Si

QUADRASORB™ Si for standard applications

• Fullyautomated,multi-sampleportanalyzerforsurfacearea,porevolumeandporesizemeasurements.Availablewithfour,threeortwosamplestations.• EachoftheanalysisportsincludesseparateandindependentDewar(coolantflask), 1000torrpressuresensorandPo(adsorbatesaturatedvaporpressure)measurementstationforsimultaneousmeasurementsyieldingmaximumthroughputandflexibility.

• EachoftheanalysisportsincludesRTDcoolantlevelsensortomaintainaconstant,smallcold-zoneformaximumsensitivity.LonglifeDewarflasksformeasurementsexceeding30hours.

• Eachanalysisportcanbeindependentlyprogrammedwithdifferentanalysesandmeasurementconditionsandnewsamplescanbestartedoneachportaspriormeasurementsarecompletedwithlittle,orno,delaytoothersamplesalreadyinprogress.

•Choosefromtwomeasurementtechniques:PatentedNOVAhelium-freemethodand classicalheliumvoid-volumemethod.Designedforanalysesusingmanydifferentgases,includingnitrogen,argon,carbondioxide,krypton,etc.

• Multiplegasdosingmethodstooptimizeanalysistimeandresolution:1.MaxiDose™ automaticallyadjustsdosesizeinresponsetosampledemand;2.Constant Dose Volume (0.1-10ccperdatapoint);and3.Delta Volume™whichaddsdatapointsinregionsoflargeuptakesocriticalporefillingisnevermissed.

• Lowmaintenance,vacuum-volumetricsystemwithtemperaturemonitoreddosingmanifold.Highvacuum/lowpressureversionavailable(seebelow).

• Windows®-basedQuadraWin™softwareprovidesforinstrumentcontrolanda comprehensiverangeofclassicalandmodernmodelsforreportingsurfaceareaandporesize.

• Widerangeofseparatelysuppliedsamplepreparationdevices(Degassers)tomeettheneedofanylaboratory(Seepage4).

Krypton/Micropore option for low surface area and micropore measurements

• AllofthefunctionsofthestandardmodelQUADRASORBSI;includeslowpressure(10torr)sensorandturbo-molecularvacuumpump.Availablewithoptionaloil-freeroughingpump.

• Performskryptongassorptionmeasurementsforverylowsurfaceareadetermination,eg.pharmaceuticalactives,powderedmetals,etc.onanyorallsamplesstations.

• Capableoflowpressureadsorptiondata(aslowas4x10-5P/Po)necessaryformorecompletecharacterizationofmicroporousmaterials,eg.zeolites,activatedcarbons,molecularsieves,etc.

Quantachrome'sQUADRASORB SISurfaceAreaandPoreSizeAnalyzerisdesignedtosatisfybusylaboratoryneedsforhighanalyticalthroughput,withoutsacrificingprecision,flexibilityorcost-effectiveness.Uptofoursimultaneousandindependent(SI)analysisportsremovethelimitationsofsingledewarsystemsallowingsamplestobestartedassoonaspreviousmeasurementsarecompleted.Thismeasurementflexibilityhasneverbeforebeenavailableinsuchacompactandcost-effectivepackage.

Transducer Accuracy:

Pressure Resolution:

Ultimate Vacuum:

Adsorbate:

Surface Area Range:

Minimum Pore Volume (liquid):

(STP):

Pore Size Range:

Coolant Level:

Minimum P/P0 (N2):

TheQUADRASORBTMSIanalyzerismicroprocessorcontrolled,andcommunicateswithaWindows®Vista,2000orXP-basedPCutilizingQuantachrome’sstate-of-the-art,dataacquisitionanddatareductionsoftware,QuadraWinTM.A21CFRPart11compliantsoftwareversionisavailableforthepharmaceuticalindustry.

State-of-the-artTheQuadraWinsoftwareispowerfulanduserfriendly.QuadraWinissuperiorfordatareduction,incorporat-ingthelatestDFT(DensityFunctionalTheory)models.Thesoftwareguidesyouthroughanalysissetup,datareduction,graphsandreportprintouts.Duringoperationonecanviewtheaccumulateddata,theisothermandallassociatedgraphsandanalyti-calresultsuptothatpoint.Afterarun,reportsandgraphsareprintedautomaticallyoryoucanusethesoftwaretodeterminethebestfittingmethod,tocomparedatabyoverlayingcurvesortoadjustgraph,size,scaling,titles,plotmarkersandlinecolorsforbestprintout.

Data presentationAcomprehensiverangeofsurfaceareaandporesizemethodsisavailable:

• Adsorptionanddesorptionisotherms.• Multi-andsinglepointBETsurfacearea.• Langmuirsurfacearea.• Mesoporesizedistributions(BJHandDHmethods).• t-methodbydeBoer,Halsey,carbonblack(STSA).•Alpha-sandMPmicroporemethods.• Totalporevolume,andaverageporesize.• Dubinin-Radushkevich(DR)microporesurfacearea.• Horvath-Kawazoe,(HK)Dubinin-Astakhov(DA)and Saito-Foley(SF)microporemethods.• ExtensiveDensityFunctionalTheory(DFT)libraryforunifiedmicro-andmesoporeanalysisusingN2, ArandCO2.• FractaldimensionbyFrenkel-Halsey-Hill(FHH)orNeimark-Kiselev(NK)models.

Transparent blue cover protects sample stations and Dewars during analysis operation. Opens vertically for easy access to analysis stations

Lower front panel opens to provide unrestricted access for Dewar placement, maintenance and clean-up

Up to four sample stations, each with coolant level sensor and Po cell

Automated, independent dewar elevators

Communication port for PC control via Windows®-based software

0.1%span(1000torrtransducer)eachmanifold/samplestation0.15%reading(10torrtransducer-optional)manifold

0.016torr(1000torrrange)0.00016torr(10torrrange)

<1x10-2torrachievedbydedicated2stagerotary,directdrivepump1x10-9torrachievedbyturbo-molecularvacuumpumpinQUADRASORBSI-KR/MP

Nitrogenoranyothernon-corrosivegaswithappropriatecoolant

0.01m2/gtonoknownupperlimit(nitrogen)0.0005m2/gtonoknownupperlimit(krypton)KR/MP-modelonly

2x10-6cc/g0.0001cc/g

3.5-4000Å/0.35-400nm

AutomaticcompensationbyRTDcoolantlevelsensor

1x10-3QUADRASORBSI4x10-5QUADRASORBSI-KR/MP

Transducer Accuracy:

Pressure Resolution:

Ultimate Vacuum:

Adsorbate:

Surface Area Range:

Minimum Pore Volume (liquid):

(STP):

Pore Size Range:

Coolant Level:

Minimum P/P0 (N2):

Analysis Specifications

*Pressuretransducerandvacuumpumpspecificationsfromtheirrespectivemanufacturers.

QuadraWinTM

- Software

Multiplegraphsshowisothermandrelatedplots

QUADRASORB™ Si

Consistentandreliablesurfacearearesultsdependuponpropersamplepreparationprocedures.IntermsofB.E.T.analysis,thelimitingstepinrateofthroughputisoftensamplepreparation.Thecompletedegassingofsamplescanoftenrequireseveralhours,whilesurfaceareameasurementsmayrequireaslittleaseightminutes.Quantachromemanufacturesseveralmodelsofdegasserstofulfillyoursamplepreparationneeds.ThesedegassersprovideavirtuallycontinuoussupplyofproperlypreparedsamplesfortheQUADRASORBSISurfaceAreaandPoreSizeAnalyzer.

Number of sample ports:

Separate temperature control for each sample port:

Temperature ramping:

Heating timer:

Software ramp control:

Analog ramp control:

Vacuum degas mode:

Vacuum display:

Flow degas mode:

Maximum temperature:

Cold trap:

Vacuum pump:

6

All ports at same temperature

No

No

No

No

N/A

N/A

Yes

400°C

N/A

N/A

6

All ports at same temperature

No

No

No

No

Yes

Yes

Yes

400°C

No

Sold separately

Autosorb DegasserThegold-standardinsampleprepa-rationforphysisorptionanalyzers.Individualtemperaturecontrolandrampratesforallsixstations,plusoptionaluseofheatertimers.Built-incoldtrapforefficientremovalofcondensablesatlowdegassingtemperaturesandforcleanvacuum.Vacuumpumpincluded.Turbo-pumpedversionavailableforrapidhigh-vacuumdegassing. MasterPrep™ Degasser Fullyfeaturedpreparationunit.IndividuallyheatedstationswithprogrammableheatingprofilesforR&D,commerciallabsandmulti-userlabora-tories.Dualmodes(vacuumorflow)forfurtherflexibilityandoptimization.TemperaturecontrolandloggingviaPCsoftware(included).Integralcoolingstationsprovideadditionalconvenience.Vacuumpumpnotincluded.

Dimensions:

Weight:

Electrical:

Environmental:

Sample Preparation: Degassers

6

Yes - with independent ovens

Yes - up to 20 steps, independent for each

sample port

Yes

Yes

No

Yes

Yes

Yes

425°C

No

Sold separately

6

Yes - with independent heating mantles

Yes - with manual adjustment, independent

for each sample port

Yes

No

Yes

Yes

Yes

No

350°C (450°C with optional quartz mantles)

Yes

Included (turbo pump optional)

MasterPrep Autosorb DegasserFeatures Flow Degasser FloVac Degasser

The FloVac™ DegasserTheFloVacprovidescosteffectivevacuumdegassing.Completewithsingle-zoneheater(to400°C),digitaltemperaturecontrollerandbuilt-indigitalvacuumgauge.Eachsamplestationhasitsownadjustableevacuation/backfillratecontrol.Flowdegassingisalsopossibleandcanbeadvantageousinremovinglargequantitiesofmoisturepriortovacuumdegassing.Individualcoolingstations.Vacuumpumpnotincluded.

Flow DegasserThepopularFlowDegasserhasthesameheatingandcoolingfeaturesastheFloVacbutwithoutvacuumcapability.Idealforqualitycontrolapplications,teachingandstart-uplabs.Eachsamplestationhasitsownadjustableflowratecontrol.

QUADRASORB™ Si

A section of one greatly enlarged particle of a solid.

1

The monolayer of adsorbed molecules; typically 15 - 20% saturation.

2

The multilayer capillary condensation stage approximately 70% saturation.

3

Total pore volume filling; approximately 100% saturation.

4

Dimensions:

Weight:

Electrical:

Environmental:

Physical Specifications

Height:29.0inches(73.6cm)HeightOpen:44.0inches(111.6cm)Width:25.25inches(63.7cm)Depth:21.0inches(53.3cm)DepthOpen:26.2inches(66.5cm)

54.4kg(120lbs.)

100-240VAC,50/60Hz

10-38°Coperatingrangeat90%maximumrelativehumidity

Accessories

Regulator AssemblyProperQuadrasorbfunctioningisassuredwhenhigh-qualitygasregulatorsareused.Quantachromesuppliescompleteassemblieswhichincludetwo-stageregulatorswithdualgauges,cylinderconnector, isolationvalveand1/8"gas lineconnector.Theregulatorsfeaturestainlesssteel,non-ventingdiaphragmsandtheappropriateCGAfittingforspecificgases.Differentassembliesareavailablefornitrogen(andotherinertsincludinghelium),hydrogen,carbonmonoxide,oxidizinggasesetc.

Vacuum Pump (standard applications).

Allvacuum-volumetricgassorptionanalyzersrequireagoodvacuumpumpandtheQuadrasorb-SIisnoexception.Thepumpshallhavethecapabilitytopullanultimatevacuumof10millitorrorbelow.Quantachromecansupplythecorrectlysizedpumpcompletewithoil,hosesandfittings.YouarenotrequiredtopurchasethenecessaryvacuumpumpfromQuantachrome,butifyoudotheentiresystemwillhavebeenqualifiedinourfactoryasaset,ensuringconsistentperformance. Vacuum Pumps (krypton/micropore model).

Lowpressureapplicationsrequireadeepervacuumthatcanonlybeachievedbyaturbo-molecularpump.Theturbopumpisincluded,andthecorrectbackingpumpcanbesuppliedbyQuantachromeeitherasarotaryoilpumporasanoil-free,drydiaphragm(membrane)pump.

Storage Dewars

Fortheconvenienceofhavinglargerquantitiesofliquefiedgasesonhand,Quantachromeoffersstoragedewarsinsizesrangingfrom5litersto30liters,plusatransferdeviceandtrolleyforthelargestsize.

The Gas Sorption Process

Beforeperforminggassorptionexperiments,solidsurfacesmustbefreedfromcontami-nantssuchaswaterandoils.Surfacecleaning(degassing)ismostoftencarriedoutbyplacingasampleofthesolidinaglasscellandheatingitundervacuumorflowinggas.Figure1illustrateshowasolidparticlecontainingcracks,orificesandporesofdifferentsizesandshapesmightlookafterpretreatment.

Onceclean,thesampleisbroughttoaconstanttemperaturebymeansofanexternalbath.Then,smallamountsofagas(theadsorbate)areadmittedinstepsintotheevacuatedsamplechamber.Gasmoleculesthatsticktothesurfaceofthesolid(adsorbent)aresaidtobeadsorbedandtendtoformathinlayerthatcoverstheentireadsorbentsurface.Basedonthewell-knownBrunauer,EmmettandTeller(B.E.T.)theory,onecanestimatethenumberofmoleculesrequiredtocovertheadsor-bentsurfacewithamonolayerofadsorbedmolecules,Nm(Figure2).MultiplyingNmbythecross-sectionalareaofanadsorbatemoleculeyieldsthesample’ssurfacearea.

Continuedadditionofgasmoleculesbeyondmonolayerformationleadstothegradualstackingofmultiplelayers(multilayers).Theformationoccursinparalleltocapillarycondensation(Figure3).ThelatterprocessisapproximatelydescribedbytheKelvinequa-tion,whichrelatesequilibriumgaspressuretothesizeofcapillariescapableofcondens-inggaswithinthem.

Astheequilibriumgaspressureapproachessaturation,theporeslargelycompletelyfillwithadsorbate(Figure4).Knowingthedensityoftheadsorbate,onecancalculatethevolumeitoccupiesand,consequently,thetotalporevolumeofthesample.Ifatthisstageonereversestheadsorptionprocessbywithdrawingknownamountsofgasfromthesysteminsteps,desorptionisothermsaregenerated.Theresultinghysteresisleadstoisothermshapesthatcanbemechanisticallyrelatedtothoseexpectedfromparticularpore-shapes.

OldercalculationmethodssuchastheonebyBarrett,JoynerandHalenda(B.J.H.)allowthecomputationofporesizesfromequilib-riumgaspressures.Onecanthereforetakeexperimentalcurves(isotherms)ofadsorbedgasvolumesversusrelativepressuresandconvertthemtocumulativeordifferentialporesizedistributions.

ModernporesizemodelsarebasedonNon-localDensityFunctionalTheory(DFT)-astatisticalmechanicsapproachthatallowsonetodescribethesorptionofgasmoleculesinnanoporousmaterialsatamolecularlevel.Hence,theapplicationofsuchmicroscopicmethodsproducesthemostaccuratesurfaceareaandporesizeresults.

QUADRASORB™ Si

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Our policy of continuous development may cause the information and specifications contained herein to change without notice or liability.

For40years,Quantachrome’sscientistsandengineershaverevolutionizedmeasurementtechniquesanddesignedinstrumentationtoenabletheaccurate,precise,andreliablecharacterizationofpowderedandporousmaterials:

• Adsorption/DesorptionIsotherms• SurfaceAreaMeasurement• PoreSizeDistribution• ChemisorptionStudies• WaterSorptionBehavior• MercuryPorosimetry• TrueSolidDensity• TappedDensity

NotonlyareQuantachromeproductstheinstrumentsofchoiceinacademia,butthetechnologyconceivedanddevelopedbyourexpertstaffisappliedinindustriallaboratoriesworldwide,whereresearchandengineeringofnewandimprovedporousmaterialsisongoing.Manufacturersalsorelyonporousmaterialscharacterizationtechnologytomorepreciselyspecifybulkmaterials,tocontrolquality,andtoisolatethesourceofproductionproblemswithgreaterefficiency.

Quantachromeisalsorecognizedasanexcellentresourceforauthoritativeanalysisofyoursamplesinourfullyequipped,state-of-the-artpowdercharacterizationlaboratory.

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© 2008 Quantachrome Corporation 0608 07160 Rev.C