ifpac conference - feb 14, 2018 chemcal, a surface cleaning … · 2018. 6. 8. · ifpac conference...
TRANSCRIPT
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IFPACConference-Feb14,2018ChemCal,asurfacecleaningvalida?ontoolfordeposi?ngpre-determined
chemicalconcentra?ons,usedinthecalibra?onofsurfacecleaningvalida?ontools.
Authors:MichaelReidWilliamHugRayReid
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• SurfaceChemicalDeposi?on:• Featuresize,resolu?onofthedepositsandnega?vespace.• Chemistryofdeposi?onandringforma?on.• Solventmorphologies:alcohols,water,acetonitrile,acetates• Solventviscosi?es.• Interleave/overlayofmul?plechemicals.• DryingpaNerns.• Unusualsubstrates:i.e.EPDM,TEFLON,screens,meshandcurvedsurfaces.
WewillbediscussingtheChemCal–asurfacechemicalprinter.
Areyouattherighttalk???
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Why?Rapidsurfacecleaningvalida?on(RCV)holdsthepromiseofreducedrelianceonswabbingandHPLC,yieldingimmediatecleaningfeedback.Ascompaniesuseon-surfacechemicaldetectorsforquan?fyingresiduestheneedtocalibratethesedeviceswithhomogenouschemicaldeposi?ontechniquesbecomesparamount.Applica?ons:Calibra?on/valida?onofnewrapidcleaningvalida?ontoolsi.eTraC.Crea?onofnewswabbingprotocols.Trainingnewswabbingpersonnel.Prin?ngknownamountsofthinlayerAPIfordrugdelivery.In-Situhotspotdetec?ontraining.ResearchonthinlayerAPIchemistrysuchassublima?on,oxida?vedamage,photo-stabilityetc.
ChemCal–asurfacechemicaldepositor.
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InkjetPrin?ng
ManualDeposi?on
ChemCalPrinter
UltrasonicPiezoPrin?ngSprayCoa?ng
Speed Uniformity
KnownQuan4ty
SpinCoa?ng
ChemCal: Status Of Deposi3on Methods
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ChemCal: Overview
TraCsensor
Opera?onalScenario:1. LoadAPIsinMicro-centrifugerack.2. Loadcouponsontotray.3. PressStart.4. Thesystemoutputsafullcalibra?oncurvein
under4hours.(Printandscan16coupons.)
Howdoesitwork?ANISTtraceablesyringeacquiressample.Then,thesyringedispensesknownmassperunitareaontoasinglecouponinanarrayformat...Repeatforeachcoupon. ChemPrinthead
Createscouponswithanaprioriknownconcentra?onsofmanydifferentchemicals,includingAPIs,detergents,excipients,etc.onPharma-typesurfacesforthepurposeofperformingcalibra?onofhand-heldTraCsensorsforrapidcleaningvalida?on.
22xVialHolder16xCouponPlaAer
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Surface Deposi3on Vocabulary
Drop–asessileliquidonasurfaceDeposit–adrysampleaaeradrophasdesiccated.Beam–theareaofalightsourcemappedontoasurface.Iwilltrynottousethewordsspotormarkorsample(ambiguity).Arealconcentra?on(microgram/cm2).Volumetricconcentra?on(microgram/microliter).
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Coffee Ring Drying PaCern
ThreeRequirementsforCoffeeRingForma4on:1. Solventmeetsthesurfaceatanonzerocontactangle(OrangeArrow).2. Contactlineispinnedatit’sini?alposi?on(GreenArrow).3. Thesolventevaporates(slowly).
DarkerPerimeter
LighterCenter
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Detailsofhowacoffeeringstainforms.
Deegan,RobertD.;Bakajin,Olgica;Dupont,ToddF.;Huber,Greb;Nagel,SidneyR.;IwiNen,ThomasA.(1997)."Capillaryflowasthecauseofringstainsfromdriedliquiddrops".Nature.389(6653):827–829.
Assumeanevenevapora?onasafunc?onofsurfacearea:Tomaintainthegeometry(i.e.pinnedouterborder)thedropletinteriormustflow(bluearrow)fromthethickcenterareatotheouterthinareatoreplenishthesolventlosttoevapora?on(green).Thisresultsinanetcompensa?ngflowofsolventfromthecentertotheperiphery,thenetoutwardsolventflowcarrieswithitsoluteand/orsuspendedpar?cles.Thisresultsinasolutesringmassthatisdispropor?onatelylargeinaerialdistribu?on.
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OtherFactorsinfluencingdryingmorphologies.
IrregularSoluteAccumula?on:Gravita?onalBuoyancyForce.Circula?ngsurfacetensiongradientdrivenflow.
RoughMorphologyCauses:
Evapora?vegradients.Shapeofsolute.Solventdryingrate.AppliedVoltage.
Images:Thermocapillaryconvec?oninliquiddroplets.NASASTIProgram.J.C.Duh,SverdrupTechnology,Inc,NASALewisResearchCenter.
Circula?ngsurfacetensiongradientdrivenflow.
Gravita?onalBuoyancyForce.
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Whydowerequiredepositswithsmallradiitoincreasehomogeneity?Varia?onofsolutesmassdistribu?onacrossanindividualdepositislarge.Generallythisiscounteredbyintra-depositinconsistenciesasvolumedecreases(Difficul?esinkeepingsmalldropsconsistent).
Issueswithlargedeposits:Op?calpenetra?onofdetectors.Swabbingremovalissues.Chemicalmodelingissuesofreac?ons:sublima?on,photo-oxida?on,autoxida?on,orstainlesssteelmediatedcatalysis.
Homogenous Non-Homogenous
MicrographCrosssec4on
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Quan?tyofdropletsinDetectorpath
ActualPrint
Polka-Do
tFish-Scale
FishScale: PolkaDot:Pinnedcontactline. De-wenngRapiddryrate. SlowdryrateLowcontactangle HighcontactangleHighsurfaceadhesion Lowsurfaceadhesion
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Wewillconsiderthreeareasofsurfacechemicaldeposi?on:1.Printquality
NISTtraceability,intra/intersamplereproducibilityaprioriknowledgeofdepositedarealconcentra?on.
2.Chemistrylimita?ons:solventcompa?bility,solventviscositylimita?ons,interleave/overlayofmul?plechemicalsanddryingpaNerns.
3.Substratecompa?bility.
Unusualsubstrates:i.e.StainlessSteel,EPDM,TEFLON,screens,meshandcurvedsurfaces.
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PrintqualityNISTtraceability.Intra&intersamplereproducibility.Aprioriknowledgeofdepositedconcentra?on.
y=31296x-282152R²=0.9846
0
500
1,000
1,500
2,000
2,500
3,000
3,500
4,000
4,500
5,000
40 60 80 100 120 140 160
Photod
iode
Signa
l(Co
unts*1000)
PercentageofTargetAPI
API-1Calibra4onCurveRange=50%to150%
100%Targetis8.48µg/cm2
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Concentra?onOrdersofMagnitude(30ng/cm2to10micrograms/cm2),
y=25369x2+2E+06x+146124R²=0.99991
100000
5100000
10100000
15100000
20100000
25100000
0 1 2 3 4 5 6 7 8 9 10
Signal(C
ounts)
Concentra?on(microgramspercm2)
Calibra?onCurve(API#072TraC_C-CH3)
20 40 80 160 320 640 1,2802,5605,12010,240
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Solventcompa?bility• DryingpaNerns.• Emptyring• Homogenousring• SmallSpot
Acetonitrile Ethanol EthanolWaterMix
MixedAlcohol EthylAcetate Methanol
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2.Chemistrylimita?ons• Solventviscosi?es
GlycerolStockSolu?onwithRedInk. Water 0.00089Pa*sEthanol 0.00109Pa*sGlycerol 0.95 Pa*s
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3.Substratecompa?bility
Considera?ons:Interplaybetweenthesurfacetensionofthedepositandadhesiontothesubstrate.Cleanlinessdeterminespinnedperimeterforsolventsthathaverecedingperimeter.SuccessfulPrintedMaterials:StainlessSteel(304,316,[#8,#7,#4])TeflonAluminumEPDMPaperQuartzPolycarbonatePVCAcrylicManymore..
Stainless316#8 TeflonAluminum EPDM
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2.Chemistrylimita?onsSecond,thechemicalinterac?onsdealwith:• Interleave/overlayofmul?ple
chemicalsSomechemicalsinteractlikesodiumhydroxideandAPIs.Yetuserswanttocombinethemwithouttouching.Presstheinterleaveop?onandenterthewellnumbers.
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Screens&mesh.(50%Stainlesssteelmeshshownhere)
Wholecoupon
Frac4onalcoupon
100% 46%
Depositaknownamountandtestyourfacili?esSwabbers!OrifyouareaNemp?ngtospincoat,tryascreen/mesh.
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Substratecompa?bilitydealswithtopographicallychallengedsubstrates:i.eCurvedsurfaces.
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Conclusion:Inconclusion,wehavegivenyouthechemicalgroundworktodebugyourdeposi?onproblemsand/orenhanceyourcurrentsurfacedeposi?onmethodologies.Ihopewehavemadeacompellingcasethatifyouarefumblingwithspincoa?ng,spraycoa?ng,ormanualdeposi?oncontactusandwecangivesomehelpwithyourdeposi?oninstrumenta?onorrapidcleaningtoolsneeds.
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Micrographs