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08855,BLENDERACETAMINOPHENPOWDERSOMEERIWITHRESPECTTOTWOAXESAHORIZONTALAXISTUMBLINGMOTION,ANDACENTRALSYMMETRYAXISSPINNINGISCONDUCTEDONMIXINGPERFORMANCEOFPOWDERSANDTHEEFFECTOFCRITICALINAMETALLTHELONGATIVELTYPEISTHETUMBLINGBLENDER,WHEREGRAINSflOWBYDEVICE,MIXINGANDSEGREGATIONMECHANISMSINTHESEDEVICESARENOTMICRONIZEDACETAMINOPHENWEUSEEXTENSIVESAMPLINGTOCHARACTERPOWDERTECHNOLOGY19620091–7CONTENTSLISTSAVAILABLEATSCIENCEDIRECTPOWDERTECHNOLOGYSFULLYUNDERSTOODANDTHEDESIGNOFBLENDINGEQUIPMENTISLARGELYBASEDONEMPIRICALMETHODSTUMBLERSARETHEMOSTCOMMONBATCHMIXERSININDUSTRY,ANDALSOfiNDUSEINMYRIADOFAPPLICATIONASDRYERS,KILNS,COATERS,MILLSANDGRANULATORS4–8WHILEFREEflOWINGMATERIALSINROTATINGDRUMSHAVEBEENEXTENSIVELYSTUDIED9,10,COHESIVEGRANULARflOWSINTHESESYSTEMSARESTILLNOTCOMPLETELYUNDERSTOODLITTLEISKNOWNABOUTTHEEFFECTOFFUNDAMENTALPARAMIZEMIXINGBYTRACKINGTHEEVOLUTIONOFACETAMINOPHENHOMOGENEITYUSINGANEARINFRAREDSPECTROSCOPYDETECTIONMETHODAFTERMATERIALSANDMETHODSAREDESCRIBEDINSECTION2,RESULTSAREPRESENTEDINSECTION3,FOLLOWEDBYCONCLUSIONSANDRECOMMENDATIONS,WHICHAREPRESENTEDINSECTION4ETERSSUCHASBLENDERGEOMETRY,SPEED,fiLLLEVLOADINGPATTERNANDAXISOFROTATIONONCOHESIVEPOWDERSORTHESCALINGREQUIREMENTSHOWEVER,CONVENTIONALTUMBLERS,ROTATINGALLSHAREANIMPORTANTCHARACTERISTICWHILE⁎CORRESPONDINGAUTHORTEL17324453357;FAX1EMAILADDRESSMUZZIOSOLRUTGERSEDUFJMUZZIO00325910/–SEEFRONTMATTER2009ELSEVIERBVALLDOI101016/JPOWTEC200906008ACOMBINATIONOFGRAVITYISAVERYCOMMONROTATIONONTHEMIXINGPERFORMANCEOFAFREEflOWINGMATRIXOFFASTFLOLACTOSEANDAVICEL102,CONTAININGAMODERATELYCOHESIVEAPI,ANDVESSELROTATIONALTHOUGHTHETUMBLINGBLENDER1INTRODUCTIONPARTICLEBLENDINGISAREQUIREDSTEPSPANNINGTHECERAMIC,FOOD,GLASS,PHARMACEUTICALSINDUSTRIESDESPITEMIXINGORPERHAPSBECAUSEOFIT,COMPARMECHANISMSINVOLVED1–3ACOMMONANDAXISOFROTATIONINTHISWORKACETAMINOPHENISUSEDASTHEACTIVEPHARMACEUTICALINGREDIENTANDTHEFORMULATIONCONTAINSCOMMONLYUSEDEXCIPIENTSSUCHASAVICELANDLACTOSETHEMIXINGEFfiCIENCYISCHARACTERIZEDBYEXTRACTINGSAMPLESAFTERPREDETERMINEDNUMBEROFREVOLUTIONS,ANDANALYZINGTHEMUSINGNEARINFRAREDSPECTROSCOPYTODETERMINECOMPOSITIONALDISTRIBUTIONRESULTSSHOWTHEIMPORTANCEOFPROCESSVARIABLESINCLUDINGTHEAXISOFROTATIONONHOMOGENEITYOFPOWDERBLENDS2009ELSEVIERBVALLRIGHTSRESERVEDVARIETYOFAPPLICATIONSURGICAL,POLYMERS,ANDHISTORYOFDRYSOLIDSYLITTLEISKNOWNOFTHEOFBATCHINDUSTRIALMIXERDIRECTIONOFROTATIONISFAST,MEDIATEDBYACONVECTIVEMIXINGPROCESS,MIXINGINTHEHORIZONTALAXIALDIRECTION,DRIVENBYADISPERSIVEPROCESS,ISOFTENMUCHSLOWERINTHISPAPER,WEEXPERIMENTALLYINVESTIGATEANEWTUMBLINGMIXERTHATROTATESWITHRESPECTTOTWOAXESAHORIZONTALAXISTUMBLINGMOTION,ANDACENTRALSYMMETRYAXISSPINNINGMOTIONWEEXAMINETHEEFFECTSOFfiLLLEVEL,MIXINGTIME,LOADINGPATTERNANDAXISOFRELATIVESTANDARDDEVIATIONNIRFUNDAMENTALPARAMETERSINCLUDINGBLENDERGEOMETRY,SPEED,fiLLLEVEL,PRESENCEOFBAFflES,LOADINGPATTERN,MIXERMOTIONADETAILEDSTUDYCOMPARINGMIXINGPERFORMANCEOFUNIAXIALAMITMEHROTRA,FERNANDOJMUZZIO⁎DEPARTMENTOFCHEMICALANDBIOCHEMICALENGINEERING,RUTGERSUNIVERSITY,PISCATAWAY,NJ,ABSTRACTARTICLEINFOARTICLEHISTORYRECEIVED17FEBRUARY2009RECEIVEDINREVISEDFORM30MAY2009ACCEPTED14JUNE2009AVAILABLEONLINE27JUNE2009KEYWORDSPOWDERMIXINGCOHESIONTHEDYNAMICSINVOLVEDINTHEORYSTILLREMAINSUNDERDEVEINMANYINDUSTRIES,INCLUDINGMIXERS”TUMBLINGMIXERSARESOMENUMBEROFREVOLUTIONSCONEBLENDERSANDBINBLENDERSMEDIATEDBYACONVECTIVEMIXINGPROCESS,ISOFTENMUCHSLOWJOURNALHOMEPAGEWWWELEL,PRESENCEOFBAFflES,MIXINGPERFORMANCEOFOFTHEDEVICESAROUNDAHORIZONTALAXIS,HOMOGENIZATIONINTHE7324452581RIGHTSRESERVEDANDBIAXIALBINBLENDERSUNITEDSTATESMIXINGREMAINSATOPICOFINTERESTFORMANYRESEARCHERS;HOWEVERTHELOPEDMOSTOFTHEMIXERSARESTILLDESIGNEDANDSCALEDUPONEMPIRICALBASISPHARMACEUTICAL,THEMAJORITYOFBLENDINGISPERFORMEDUSING“TUMBLINGHOLLOWCONTAINERSWHICHAREPARTIALLYLOADEDWITHMATERIALSANDROTATEDFORCOMMONEXAMPLESINCLUDEHORIZONTALDRUMMIXERS,VBLENDERS,DOUBLEINALLTHESEMIXERSWHILEHOMOGENIZATIONINTHEDIRECTIONOFROTATIONISFAST,PROCESS,MIXINGINTHEHORIZONTALAXIALDIRECTION,DRIVENBYADISPERSIVENTHISPAPER,WEEXPERIMENTALLYINVESTIGATEANEWTUMBLINGMIXERTHATROTATESEVIERCOM/LOCATE/POWTEC2MATERIALSANDMETHODSTHEMATERIALSUSEDINTHESTUDYARELISTEDINTABLE1,ALONGWITHTHEIRSIZEANDMORPHOLOGYACETAMINOPHENISBLENDEDWITHCOMMONLYUSEDEXCIPIENTSANDISUSEDASATRACERTOEVALUATETHEDEGREEOFHOMOGENEITYACHIEVEDASAFUNCTIONOFNUMBEROFREVOLUTIONSACETAMINOPHENISONEOFTHEDRUGSMOSTWIDELYUSEDINMIXINGSTUDIES,ANDAVICELANDLACTOSEARECOMMONLYUSEDPHARMACEUTICALTHEEXPERIMENTALPLANUSEDINTHISSTUDYISASFOLLOWSFILLLEVELBLENDER1–60FILLLEVELBLENDER2–60,70,80LOADINGPATTERNBLENDER1SIDE–SIDELOADING,TOP–BOTTOMLOADINGLOADINGPATTERNBLENDER2SIDE–SIDELOADING,TOP–BOTTOMLOADINGSPEEDBLENDER1–15RPM,20RPM,25RPMSPEEDBLENDER2ROTATIONAL/SPINNING15/75RPM,20/10RPM,30/15RPMSAMPLINGTIMEBLENDER1,BLENDER2–75,15,30,60,120REVOLUTIONS3RESULTSTHEHOMOGENEITYINDEXUSEDISTHERSD,WHERECISTHECONCENTRATIONOFEACHINDIVIDUALSAMPLE,C_ISTHEAVERAGECONCENTRATIONOFALLSAMPLESANDNISTHETOTALNUMBEROFSAMPLESOBTAINEDATAGIVENSAMPLINGTIMERSDSC;WHERESffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiNPC2−PC2NN−1SWEEXAMINETHEEFFECTOFfiLLLEVELONMIXINGPERFORMANCE2AMEHROTRA,FJMUZZIO/POWDERTECHNOLOGY19620091–7EXCIPIENTSINTHEINTERESTOFBREVITYTHEIRSEMIMAGESARENOTINCLUDEDINTHISPAPER,BUTCANBEFOUNDIN“HANDBOOKOFPHARMACEUTICALEXCIPIENTS”21NEARINFRAREDSPECTROSCOPYACETAMINOPHENHOMOGENEITYWASQUANTIfiEDUSINGNEARINFRAREDSPECTROSCOPYACALIBRATIONCURVEWASCONSTRUCTEDFORAPOWDERMIXTURECONTAININGINAVERAGE35AVICELPH102,62LACTOSEAND3ACETAMINOPHENNEARINFRAREDNIRSPECTROSCOPYCANBEAUSEFULTOOLTOCHARACTERIZEACETAMINOPHENSAMPLESAREPREPAREDBYKEEPINGTHERATIOOFAVICELTOLACTOSERANDOMIZEDINORDERTOMINIMIZEEFFECTSOFIMPERFECTBLENDINGOFEXCIPIENTSDURINGTHEACTUALEXPERIMENTSONTHEACCURACYOFTHERESULTSTHERAPIDCONTENTANALYZERINSTRUMENTMANUFACTUREDBYFOSSNIRSYSTEMSSILVERSPRING,MDANDVISIONSOFTWAREVERSION21ISUSEDFORTHEANALYSISTHESAMPLESAREPREPAREDBYWEIGHING1GOFMIXTUREINTOSEPARATEOPTICALSCINTILLATIONVIALS;KIMBLEGLASSINCVINELAND,NJUSINGABALANCEWITHANACCURACYOF001MGNEARIRSPECTRAARECOLLECTEDBYSCANNINGINTHERANGE1116–2482NMINTHEREflECTANCEMODEPARTIALLEASTSQUAREPLSREGRESSIONISUSEDINCALIBRATIONMODELDEVELOPMENTUSINGTHESECONDDERIVATIVEMATHEMATICALPRETREATMENTTOMINIMIZETHEPARTICLESIZEEFFECTSASSHOWNINFIG1,EXCELLENTAGREEMENTISACHIEVEDBETWEENTHECALIBRATEDANDPREDICTEDVALUES22BINBLENDERSUSEDINTHISSTUDYUNIAXIALBLENDERBLENDER1,BIAXIALBLENDERBLENDER2DUETOITSWIDESPREADUSE,ACYLINDRICALBLENDER1WITHACAPACITYOF30LISCHOSENASAREFERENCEBLENDERINTHESTUDYASSHOWNINFIG2,THISBLENDERHASACIRCULARCROSSSECTIONANDTAPERSATTHEBOTTOMITCANBEUSEDWITHORWITHOUTBAFflES,WHICHAREMOUNTEDONAREMOVABLELIDINTHISSTUDYALLTHEEXPERIMENTSARECONDUCTEDWITHOUTTHEUSEOFBAFflESMIXINGPERFORMANCEINTHISDEVICEISUSEDTOPROVIDEABASELINEFOREVALUATINGTHEMIXINGPERFORMANCEOFANEWLYDEVELOPEDBLENDER2WITHACAPACITYOF40L,WHICHISALSOCYLINDRICAL,INORDERTODETERMINETHEEFFECTOFDUALAXISOFROTATIONONMIXINGPERFORMANCETHEBLENDERSHOWNINFIG2BHASTWOAXISOFROTATIONTHESPINNINGRATEOFPRECESSIONRELATIVETOTHECENTRALAXISOFSYMMETRYISGEAREDTOBEHALFOFTHATOFTHERATEOFROTATIONAROUNDTHEHORIZONTALAXIS23EXPERIMENTALMETHODTWOTYPESOFINITIALPOWDERLOADINGUSEDINTHEEXPERIMENTSTOP–BOTTOMLOADINGANDSIDE–LOADING,WHICHARESCHEMATICALLYREPRETABLE1MATERIALSSTUDIEDINTHISPAPERNAMESIZEANDMORPHOLOGYVENDOR,CITY,STATEFASTFLOLACTOSE∼100Μ,SPHERICALFOREMOSTFARMS,NEWARK,NJAVICELPH102MICROCRYSTALLINECELLULOSE∼90Μ,NEEDLELIKEFMC,ROTHSCHILD,WIACETAMINOPHEN∼40Μ,NEEDLELIKEMALLINCKRODT,STLOUIS,MOSENTEDINFIG3TOAVOIDAGGLOMERATION,THEAPI,ACETAMINOPHEN,WASDELUMPEDPRIORTOLOADINGITINTOTHEBLENDERBYPASSINGITTHROUGHA35MESHSCREENINORDERTOCHARACTERIZEMIXINGPERFORMANCE,AGROOVESAMPLERWASUSEDTOEXTRACTSAMPLESFROMTHEBLENDERSAT75,15,30,60,120REVOLUTIONSTHETHIEFWASCAREFULLYINSERTEDINTHEBIN,ANDACOREWASEXTRACTEDATEACHPOINTOFINSERTIONEACH“STAB”MINIMIZINGPERTURBATIONTOTHEPOWDERBEDREMAININGINTHEBLENDERAPPROXIMATELY7SAMPLESARETAKENFROMEACHTHIEFSTAB,ANDATOTALOFfiVESTABSAREUSEDATEACHSAMPLINGTIME,ASSHOWNINFIG4SOATOTALOF∼35SAMPLESARETAKENATEACHSAMPLINGPOINTPREVIOUSLYTHEREHAVEBEENSTUDIESONTHEEFFECTOFfiLLLEVELINTHEBOHLEBINBLENDER,GALLAYBINBLENDERANDVBLENDERANDDOUBLECONEBLENDER11–13ALLTHEAFOREMENTIONEDBLENDERSHAVEONLYONEAXISOFROTATION,THEREFORETHEOBJECTIVEOFTHISSTUDYISTOEXAMINEHOWDUALAXISIMPACTMIXINGPERFORMANCESATHIGHfiLLLEVELSTOAVOIDREPETITION,STUDIESFORfiLLLEVELARENOTCONDUCTEDFORBINBLENDER1RESULTSAVAILABLEFROMAPREVIOUSSTUDYUSINGMGSTASATRACERSHOWEDTHATMIXINGINAUNIAXIALBLENDERSLOWEDDOWNQUITEDRAMATICALLYASTHEfiLLLEVELEXCEEDED70MOREOVER,RESULTSFORACETAMINOPHENCANBEASSUMEDTOBESIMILARTOTHOSEOBTAINEDINPREVIOUSWORKBYMUZZIOETAL11,13,FORASINGLEAXISRECTANGULARBINBLENDER11,WHICHHAVESHOWNTHATEVENAFTERFEWHUNDREDREVOLUTIONSHOMOGENEITYACHIEVEDWITHA80fiLLLEVELISVERYPOORASCOMPAREDTO60fiLLLEVELTOEXAMINETHEEFFECTOFfiLLLEVELINADUALAXISBLENDER,EXPERIMENTSWEREPERFORMEDINBLENDER2WITHTHETOPBOTTOMLOADINGPATTERNFORAROTATIONALSPEEDOF15RPMANDWITHSPINNINGSPEEDOF75RPMTHEfiLLLEVELSEXAMINEDARE60,70AND80RESPECTIVELYANDSAMPLESARETAKENAFTER75,15,30,60,120REVOLUTIONSTYPICALRESULTSARESHOWNINFIG5,WHICHSHOWSTHERSDVSNUMBEROFBLENDERREVOLUTIONSASEXPECTEDFORNONAGGLOMERATINGMATERIALS,THECURVESFIG1NEARINFRAREDNIRSPECTROSCOPYVALIDATIONCURVETHEEQUATIONUSEDTOPREDICTACETAMINOPHENCONCENTRATIONISVALIDATEDBYTESTINGSAMPLESWITHKNOWNAMOUNTSOFACETAMINOPHENCONCENTRATIONTHEYAXISREPRESENTSTHECONCENTRATIONCALCULATEDFROMTHEEQUATIONANDTHEXAXISREPRESENTSTHEACTUALCONCENTRATIONTHUSAPERFECTLYSTRAIGHTLINEAT45WOULDREPRESENTTHEBESTCALIBRATIONMODELEACHPOINTONTHEGRAPHREPRESENTSASINGLESAMPLETHECONCENTRATIONOFACETAMINOPHENEXAMINEDHERERANGESFROM0TO8FIG2PICTORIALREPRESENTATIONOFABINBLENDER1ANDBBINBLENDER2SHOWINGTHECORRESPONDINGAXISOFROTATIONFIG3SCHEMATICOFTHELOADINGPATTERNUSEDINTHESTUDYINTOP–BOTTOMLOADING,AVICELISLOADEDfiRSTINTOTHEBLENDERFOLLOWEDBYLACTOSEONTOPOFITANDfiNALLYACETAMINOPHENISUNIFORMLYSIEVEDOVERINSIDE–SIDELOADINGAVICELISPLACEDATTHEBOTTOMANDTHENACETAMINOPHENISONLYSIEVEDONLYINHALFPARTOFTHEBLENDERANDISSANDWICHEDBETWEENLACTOSEANDAVICELFIG4ATHIEFSAMPLERBTOPVIEWOFTHESAMPLINGPOSITIONSCHEMEFIG5MIXINGCURVESFORDIFFERENTfiLLLEVELSINBLENDER2THERSDOFACETAMINOPHENISPLOTTEDASAFUNCTIONOFNUMBEROFREVOLUTIONSTHELOADINGPATTERNINTOPBOTTOMANDTHEBLENDERROTATIONALSPEEDIS15RPMWITHSPINNINGSPEEDOF75RPM3AMEHROTRA,FJMU
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