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PACKEDBEDFLUIDDYNAMICSANDAMMONIAABSORPTION

INSTRUCTIONSFORSTUDENTS

Safety
Overview
Scenario
Apparatus
Procedure
AmmoniaRotameterCalibration
Report
NotesonGasAbsorption
ResidenceTimeDistributionTheory
SampleCalculationofPressureDrop
References
Comments

A.SAFETY

1.AMMONIAISBOTHTOXICANDCOMBUSTIBLE.Ifamajorammonialeakdevelops,evacuatethe
laboratoryimmediately,withoutattemptingtoshutoffthecylindervalve.Openthemaincylindervalveonly
aboutonehalfturn,topreventdischargeathighrates.

2.Wearsafetyglassesatalltimes.Besurethelabventilationsystem(inRoom171)isoperatingbeforeusing
ammonia.Besuretheammoniacylindervalveisclosedbeforeendingtheexperiment.Knowthesafety
showerandeyewashstationlocations.

3.Wearjeansorslacks,alongsleevedshirt,andsturdyshoesthatgivegoodtractiononpossiblywetfloors.

4.Guardagainstelectricalhazardsbymakingsurethatallequipmentiswellgroundedusingthreewireplugs
andothermeans.

5.Handlewithgreatcareanysolventsorotherpotentiallyvolatile,flammable,toxic,orotherwisedangerous
chemicals.Inthisexperimentair,water,ammonia,andasolutionofpotassiumchlorideareused.Potassium
chlorideistoxicifingestedinlargeamounts.Ammoniaistoxicinhigherconcentrations.

6.Guardagainstfalls,burns,cuts,andotherphysicalhazards.Useheavyglovestoopenorclosehotsteam
orcondensatevalves.

7.THINKFIRSTOFSAFETYINANYACTIONYOUTAKE.Ifnotcertain,asktheTAorafaculty
memberbeforeyouact.

B.OVERVIEW

Thepackedbedabsorberusedinthisexperimentmaybeoperatedinthreemodes:

(a)Thepressuredropacrossthecolumnisdeterminedasafunctionofairandwaterflowrates.

(b)Theresponsetoimpulseinjectionofaninerttracerisusedtodeterminethewaterholduponthepacking.

(c)Thecolumnisoperatedatthesteadystateasanammoniaabsorber,andtheheightofatheoreticalplateis
determinedasafunctionofairandwaterflowrates.

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Ingeneral,severallabsessionsareneededtoexploreallofthesemodes.

C.SCENARIO

Packedcolumnsarecommonlyemployedtocarryoutabsorptionandscrubbingoperations.Theyprovidea
mediuminwhichcountercurrenttwophaseflowoccurs,andinwhicharelativelylargegasfluidinterface
perunitvolumeofcolumnvolumeexists.Becauseofthenatureofthepackingmaterial(oftenaceramic)a
packedcolumncanoperateusingstronglycorrosivefluids.Packedcolumnsareoftenmoreeconomicalto
buildandoperatethantheirplateorbubblecapcolumncounterparts,althoughpressuredropscanbehigh,
whichrequireslargergasblowerswithhighenergyconsumption.

Thepackedbedabsorberinthisexperimentistobeusedeventuallytoremoveammoniafromawasteair
stream.Beforerunningammonia,however,itisnecessarytodeterminewhatwaterandairflowratescanbe
accommodated,tomeasurethepressuredropacrossthebedsothattheairblowercanbespecified,andto
testanoninvasivemethodformeasuringtheamountofwaterhelduponthepacking,sothatincipient
floodingcanbedetected.

Anairstreamfromadriercontainsroughly0.10%byweight(1000ppm)ammonia.Environmental
regulationsprohibitdischargeoftheammoniaintotheair,andthusasmallpackedbedscrubberhasbeenset
uptopilottheammoniaremovalprocess.Yourjobistorunthescrubberatvariousairflowandwaterflow
rates,andcollectdatafromwhichcanbecalculatedtheheightofatransferunitforthepackingusedinthe
scrubber.Theresultswillbepassedtoadesigngroupwhichwilldesignafullscalescrubber,basedontheair
flowratefromthedrierandthemaximumallowableammoniacontentoftheeffluentair.

Yourjob,asagroup,istosetforthandcarryoutaseriesofpressuredrop,tracerresponse,andammonia
absorptionexperimentsthatwillprovidedata,andresultsderivedfromthedata,thatserveasagoodbasisfor
thedesignofafullscalescrubber.

D.APPARATUS

Thepackedcolumn(seeFig.1)consistsofa4"IDby36"longsectionofborosilicatepipesittingona4"by
2"borosilicatewell.Stainlesssteeltop,bottomandsideplatesaresealedwithTeflongasketsandprovided
withair,water,sampleandpressuretapconnections.About30inchesofceramic3/8"Raschigringpacking
issupportedabovetheairentrypoint.Thewatereffluentlineis1/2"stainlesstubingwithSwagelockfittings
thatpermittheleveloftheexitline,andthusthelevelofthewaterinthecolumnbottom,tobeadjusted.

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Waterenteringthetopofthecolumnisdistributedevenlyoverthepackingbya4armdistributor.Theair,
water,andammoniafeedratesaresetmanuallyandmeasuredbyrotameters.Awatermanometerisusedto
measurethepressuredropacrossthepacking.Aninfraredammoniaanalyzersamplestheeffluentairstream
andindicatestheammonialevel,typically50to1000ppm,inthisstream.Thesignalfromthisanalyzeris
acquiredbyaA/DboardmountedinamicrocomputerandprocessedbyaLabVIEWprogram.

ThepackingconsistsofceramicRaschigrings,length3/8inch,width3/8inch,wallthickness1/16inch,
weight51lbs/cubicfoot,equivalentsphericaldiameter0.35inch,0.68voidfraction,surfacearea134sq
feet/cubicfoot.

Asyringeisusedtoinjectpotassiumorsodiumchloridesolutionatthetoporbottomofthecolumn.
Typically10mlof0.2MKCltracerisinjected.Thetracerconcentrationismeasuredbyaconductivitycell
locatedinthewatereffluentline,thecellbeingconnectedtoaYSIconductivitymeter.Thesignalfromthe
meterisacquiredbyaLabVIEWprogramviaaNationalInstrumentsA/Dboard.Fromtheresponseto
impulsetracerinjectionthevolumeofwaterbetweentheinjectionpointandmeasurementpointmaybe
calculated.

Regulatorsaremountedinwaterandairsupplylinesinordertoreducetheeffectofsupplypressure
variationsontheflowrates.Ifthesupplypressuresarerelativelyconstanttheseregulatorsmayberemoved.

E.PROCEDURE

Inspection

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Theapparatusshouldbeexaminedcarefully.Checkthattheeffluentwaterlinefromthecolumnisoverthe
drainandthat,ifammoniaistobeused,theeffluentairentersthelaboratorychemicalhoodsystem.Theball
valvesonthetracerinjectionlinesshouldbeclosed.Theairpressureregulatorshouldread20to40psig.
Notethattheairrotameteroperatesatessentiallyatmosphericpressure,regardlessoftheregulatorsetting.

CalibrationoftheWaterFlowRotameter

Withtheairflowoff,setthewaterflowratetoalowvalueusingthewaterrotameter(readthecenterofthe
ball),andrecordthetimeneededtocollect250mlofeffluentwater.Adjustthewaterexitlinelevelif
necessarytoproduce5to10cmofwaterinthebottomofthecolumn.Thenincreasethewaterflowratein
about6incrementsovertherangeavailable,measuringit(inml/min)ateachsetting.Thewaterrotameteris
nowcalibrated.

DryColumnPressureDrop

Withnowaterflowbutwithawatersealinthewatereffluentline,settheairflowrateateightortenevenly
spacedpointsontheairrotameter,withamaximumratetypically6to10scfm.Ateachsteadystatethe
pressuredropacrossthedrypackingshouldbemeasuredusingthewatermanometer.Afterthefinalhigh
pressuredrophasbeenrecorded,theprocessshouldbereversedanddatashouldbetakenatdecreasingair
flowratesoverthesamerange.Fromthesedataadrycolumnpressuredropvs.airflowrateplotcanbe
constructed.

PressureDropasaFunctionofAirandWaterRates

Forarangeofwaterflowratesandairflowrates,allowthecolumntocometosteadystateandmeasurethe
pressuredropusingthewatermanometer.Atthehigherwaterandairflowratesyoumayseeflooding,i.e.a
continuingaccumulationoflargeamountsofwateronthepacking,coupledwithaveryhighpressuredrop
(whichmayblowtheliquidsealatthebottomofthecolumn).Infullfloodingasteadystatewillnotbe
possible.Takedatathatdefinetheairrate/waterrateregionthatproducesfloodingaswellaspossible.Atair
flowratesbelowfloodingthetimeconstantofthecolumnisquiteshort,ontheorderof10to30seconds,so
thatmanyrunscanbemadeinarelativelyshorttime.

Pleasereportyourresultsinthefollowingunits:length=ft,volume=ft3,time=seconds,mass=pounds
mass(lbm)andmassflux=lbm/(ft2s).

LiquidHoldupMeasurement

Atagivensteadystate,theliquidholdupcanbemeasuredbyanindicatordilutiontechnique.Usinga
syringe,10mlof0.2NKClisinjectedrapidlyintoeitherthetoporbottominjectionport(Notethattracer
concentrationmaybevariedtogivethebestresponse,andthatNaClorNH4Clmayalsobeusedastracers).
Theconductivityofthewaterexitingfromthecolumnismeasuredusingtheconductivitymeterandrecorded
asafunctionoftimeusingacomputerbaseddataacquisitionsystem.

ThecomputerusedwiththeexperimentisaPentiummachine.WeassumethatdirectoryZZQB45containsa
recentversionofMicrosoftQuickBASIC,andthatprogramTRACER04.BASisinZZQB45.Afterbooting
thecomputer,attheDOSprompttypeCD\ZZQB45toconnecttoZZQB45,andthentypeQBTRACER04.
Thisloadstheprogram.NowhitALTRtoruntheprogram,andfollowtheinstructionsissuedbythe
program.Theprogramwillcollectbaselinedata,andthencallfortheinjectionoftracer.Usually10mlof0.2
MKCltracerisinjected.

AlternatelyaNationalInstrumentsLabVIEWprogramwillbeusedtoacquire,plot,andprocessthetracer
responsedata.

Fromthedataontracerconcentrationasafunctionoftimethemeanresidencetimecanbedetermined,as
discussedinsectionHbelow.Sincethewaterflowrateisknown,thewatervolumebetweentheinjectionand
measurementpointscanbefound.Thentheholduponthepackingisfoundbydifference.Notethatthese
calculationsaredonebytheprogram,andcanalsobedonebyloadingthedatawrittentoafilebythe
programintoaspreadsheet,e.g.EXCEL.

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Severaltracerinjectionrunsshouldbemade,someathigherairandwaterflowratesthatproducesignificant
holdup.Typically,atahighwaterflowrate,severaldifferentairflowrateswouldbeused,thelast
correspondingtoincipientflooding,i.e.toalargeholdupofwateronthepacking.Duringtheserunsthe
waterexitlineshouldbeadjustedtogiveminimalwaterlevelinthecolumnbottom,say2to4cm.Butbe
surethatnoairleavesthewatereffluentline,i.e.thatthewatersealatthebottomofthecolumnisnotlost.A
lostsealcanberecoveredbyturningdowntheairflowrateforashorttimeandallowingthewaterdischarge
linetofill.

Youcanverify,atleastroughly,theholdupdeterminedasabovebyshuttingoffthewaterflowuntilasteady
stateisreached,measuringtheincreaseinwaterlevelinthecolumnbottom,andcollectingthewaterthat
drainsfromthecolumnfollowingwatershutoff.

AmmoniaAbsorption

oTurnontheMSAanalyzerandallowtowarmupfor30minutes.Theanalyzershoulddrawaroomair
sample.Zerotheanalyzermeterusingthecontrolprovided.

oOpentheammoniacylindervalveabout1/2turn,settheregulatorpressureto20psig,openanyvalves
betweentheregulatorandtherotameterwide,adjusttherotametervalvetoproduceareadingof150atthe
centeroftheball.Optionally,opentherotametervalvefurthertoproducealargerflowofammonia,andthus
alargereffluentammonialevel.(IfnecessaryCAREFULLYcheckforammonialeaksusingamodified
squeezebottleofmoderatelyconcentratedHCluseeyeprotection!tosprayastreamofHClontubing
jointsandvalvepacking.)

oSetabaseairflowrateandammoniaflowrate,asindicatedbytherotameters.Withnowaterflow,allow
thecolumntocometosteadystateandnotetheanalyzerreading.

oConverttheairflowratefromSCFMtogmol/minandcalculatetheammoniaflowrateingmol/minfrom
theammoniarotametercalibrationdata(fullscaleis329standardcc/minat20psigpressureinthe
rotameter).Fromthesevaluescalculatetheammonialevelintheairfeedstream.(Notethatasamplingpoint
couldbeaddedtotheair+ammoniafeedline,butthattheammonialevelatthispointmay,atlowairflow
rates,exceedthe1000ppmmaximuminputtotheanalyzer.Ifthecolumnisrundry,afterafewminutesthe
ammonialevelintheeffluentairwillequalthefeedlevel,andtheanalyzerwilldisplaythislevelifitisless
than2000ppm.)

oSet(andthenmonitor)thedesiredNH3,airflow,andwaterflowrates.Connecttheanalyzertotheeffluent
gasstream,recordtheanalyzerreading(assumedtobemolefraction).Taketheammoniarotameterreading
whenasteadystatehasbeenachieved,whichshouldtakeabout5minutes.

oRecordthepressuredropacrossthepackedcolumn.

oBasedontheattachednotes,calculatethenumberoftransferunits(NTU)andtheheightofatransferunit
(HTU).

oRepeattheabovestepsforcombinationsofwaterflowratesandairflowrates.Combinationsleadingto
floodingshouldbediscarded.Theammoniafeedrateshouldbesuchthatmeasurableammoniaispresentin
theeffluentair.

Anammoniamassbalance,usedtofindxB,is

Lx0+VyF=LxB+Vy1

Withx0=0,wehave

xB=(V/L)(yFy1)

whereVisthevaporrate(g/min)andListheliquidrate(g/min).

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F.AMMONIAROTAMETERCALIBRATION

UsethevalveprovidedtopassNH3fromtherotameterthroughafrittedglassabsorptiondeviceintoanHCl
solution(ofsuitableconcentration)containingphenolphthalein.Findthetimeneededtoneutralizeallthe
HCl.Fromthedataobtained,findtheflowrateofNH3atseveralrotametersettings.

G.REPORT

Showthecalibrationcurveforthewaterrotameter.Plotthepressuredrop(inchesH20)asafunctionofair
flowrate(SCFM)onaloglogplot,withwaterflowrateasaparameter.Includethedrypackingdata.Note
that,ifpressuredropvariesasthesquareofairflowrate,astraightlinewithaslopeof2shouldbeobtained.
Departure(inthedirectionofhigherpressuredrop)fromthecurvedefinedbythelowairflowpointsmay
indicateflooding.Leva(seereferencebelow,page28,Figure10)providesdataforasimilarcolumn.
CompareyourresultsalsowiththecorrelationinPerry'sHandbook.

Presentanddiscusstheresultsoftheindicatordilutionmeasurements.Provideacompletesamplecalculation
foratleastonerun,includingplotsoftracerconcentrationvs.timefortopandbottominjections.Usearun
inwhichtheliquidholdupwasrelativelylarge.Doesthewaterholduponthepackingincreasesignificantly
asthefloodingpointisapproached?

Fortheammoniaabsorptionruns,calculateforeachruntheheightofatheoreticalplate,anddiscusshowthis
varies(ifatall)withtheairandwaterflowrates.

Clickhereforguidelinesforthewrittenandoralreports.

H.NOTESONGASABSORPTION

Asthecarriergasmovesupthecolumnthesolutegastransfersfromthecarriergastothedescendingliquid.
Letrbetherateoftransferingmol/mincm,andletzbethedistancefromthebottomofthecolumnincm.
Thenwehave(seedrawingbelow)

Vdy/dz=r

and

Ldx/dz=r

whereVandLare(assumedconstant)vaporandliquidrates(gmol/min),andyandxarethegasphaseand
liquidphasemolefractions.Wecandefinethemasstransferrateas
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r=k[yy*(x)]

wherey*(x)isthegasphasemolefractioninequilibriumwiththeliquidphasemolefractionx,andkisa
masstransfercoefficient.Forthegasphasewehave

dy/dz=(k/V)(yy*)ordy/(yy*)=(k/V)dz

or,integratingfromz=0toz=zF,

Theintegralontherightisameasureofthedifficultyoftransferringsolutegasthesmallerthedrivingforce
yy*,thelargertheintegral,whichwecallthenumberoftransferunits(NTU).Inordertoevaluatethe
integralwemustfindx(y)andthusy*(x(y)).x(y)followsfromasolutebalancearound,say,thetopofthe
column.Inparticular,wehavetheoperatinglineequation

LxB+Vy=Lx+VyB

or

x=(V/L)(yyB)

when,asisusual,xB=0.Theintegrand

[yy*((V/L)(yyB))]1

canbeevaluatedintermsofywhenthevaporliquidequilibriumfunctiony*(x)isknown.Wheny*=KHx,
theintegralcanbefoundanalytically.(KHistheHenry'sLawconstant.)FromzFandNTUtheheightofa
transferunit(HTU)isfound.

SampleCalculation

Airflowrate=7.0cfmat70Fand1atm

Waterflowrate=500ml/min

xB=0

NH3inairfeed=20,000ppm(calculatedfromairandNH3flowrates)

NH3ineffluentair=250ppm(fromAnalyzer)

V=7(ft3/min)(28.32L/ft3)(gmol/22.4L)(492/530)=8.125gmol/min

L=500(ml/min)(1g/ml)(1gmol/18g)=27.8gmol/min

yA=(20,000/17)/(1,000,000/29)=0.03400

yB=(250/17)/(1,000,000/29)=0.00043

AssumingT=50F,fromPerrywehavethatthepNH3over0.05molefractionaqueousammonia=0.47psia,
whichgivesy=0.47/14.7=0.0319molefractionammonia.Thus

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KH=y/x=0.0319/0.050=0.638

Fortheoperatingline

x=(V/L)yyB=0.296y0.00043

and

yy*=yKHx=y0.638(0.296y0.00043)

or

yy*=0.811y+0.000274

WenowhaveforNTU,usingMATHEMATICAorproceedinganalytically,

whichseemsreasonable.TheMATHEMATICAexpressionwhichcarriesouttheintegrationanalyticallyis

Integrate[(0.811y+0.000274)1,{y,0.00042,0.03400}]

I.RESIDENCETIMEDISTRIBUTIONTHEORY

Withoutderivingthetheory,weconsideranimpulseinjectionofaninerttracerintoaflowsystem(wellor
poorlymixed)withvolumetricflowrateQandvolumeV.Wecansay,first,thatallthetracerinjectedmust
leaveeventually.Second,allthefluidinthesystemattimezeromusteventuallybewashedoutandreplaced
bynewfluid.Thesestatementscanbeshowntocorrespondtotheequations

and

whereC(t)istheconcentrationoftracerintheeffluentfollowingtheinjectionofamountDoftraceratthe
systeminletattimet=0.Also,V/Qisthemeanresidencetimeoffluidinthesystem.NotethatCmaybe
replacedinthesecondequationbyamultipleofC,saykC,withoutaffectingthemeanresidencetimeV/Q.
FromV/Q,ifQisknown,wecanfindV.Forevenlyspacedeffluentconcentrationdatawecanusenumerical
integration,saySimpson'sRule,tofindV/Q,asshowninthefollowingexample,whereWdenotesthe
Simpson'sRuleweights(1424....241).

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Time Conc. Weight WC tC(t) WtC(t)


t C(t) W
0 2 1 2 0 0
2 4 4 16 8 32
4 5 2 10 20 40
6 2 4 8 12 48
8 1 1 1 8 8
Sums 38 128

Then,usingSimpson'sRule[(Dt/3)(142424....241)],withDt=2,

and

IfQ=200ml/min,thesystemvolumeVis200*3.368=673.6ml.Suchcalculationscanbedoneeasily
usingaspreadsheetiftandC(t)aregivenatevenlyspacedtimes.

AnalternatetoSimpson'sRuleistrapezoidalrulenumericalintegration,[(Dt/2)(1222...21)],whichcan
beusedwithasmalllossinaccuracy.

J.SAMPLECALCULATIONOFPRESSUREDROP

InPerry'sHandbook(FifthEdition,Figure1839)wehaveaplotinwhichtheabscissaXis

X=(L/G)(rg/rL)0.5

andtheordinateYis

Y=G2Fpfm0.2/(rgrLg)

HereListheliquidmassflux(lbm/ft2s)basedontheareaoftheemptycolumn,Gisthegasmassflux
(lbm/ft2s),fistheratioofthedensityofwatertotheliquiddensity,FpisapackingfactorfoundinPerry
Table185(ft1),rgisthegasdensity(lbm/ft3),rListheliquidmassdensity(lbm/ft3),mistheliquid
viscosity(centipoises),andgistheaccelerationofgravity(32.2ft/s2).NotethatYisnotdimensionless.

Asanexample,consideranairflowrateof6.0ft3/minatSTP,awaterflowrateof1200g/s,andacolumn
IDof4inches(correspondingtoacolumnareaof0.0872ft2),
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G=((6*29)/(359*60))(1/0.0872)=0.0926lbm/ft2s

L=1200/(453.6*60*0.0872)=0.506lbm/ft2s

m=1.0centipoise

Fp=1000(1/ft)

f=1

rL=62.3lbm/ft3

rg=(29/359)(273.2/298.2)=0.0740lbm/ft3

and

X=(0.506/0.0926)(0.0740/62.3)0.5=0.188

Y=(0.09262*1000*10.2)/(0.074*62.3*32.2)=0.0578

BasedonFigure1839inPerry,thegasphasepressuredropperfootofpackingisabout1.40inchesofwater.
Ifthepackingheightis30inchesthepredictedpressuredropis3.5inchesofwater.

K.REFERENCES

1.Leva,Max.TowerPackingsandPackedTowerDesign,2ndEdition,U.S.StonewareCompany,Akron
Ohio(1953).

2.Perry,J.H.,Editor.ChemicalEngineersHandbook,5thEdition,McGrawHillBookCompany,pp.2119
(1973).

3.McCabeandSmith.UnitOperationsofChemicalEngineering,3rdEdition,pp.709715(1976).

L.COMMENTS

1.Useastripchartrecorder(ifavailable)torecordtheanalyzeroutputsignal.Therecordertracecanbeused
toseewhetherasteadystatehasbeenachieved.

2.Besuretoturnofftheammoniacylindermainvalvewhentherunsarecomplete.Alsoclosetheregulator
outletvalve,butnottootightly.

3.Positionanelephanttrunkconnectedtothelaboratoryventilationsystemnearthewatereffluentcollection
point,andmakesurethelaboratoryventilationblowerison.

4.Ammonia/watervaporliquidequilibriumdataatvarioustemperaturesareavailableinPerry'sHandbook.
FromthesedataaHenry'sLawconstantcanbederived(seesamplecalculationabove),andthisisusedinthe
NTUcalculation.Useathermometertomeasuretheeffluentwatertemperature.

5.Checktheammoniacylinderpressuregaugebeforeandaftertherun.Itshouldshow80to120psig.A
lowerpressuremeanstheammoniacylindercontainsnomoreliquid,andtheTAorafacultymembermust
beinformed.

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