Lab32:

WhatisinthisContainer:ACapstoneExperiment
KadelynEgan,ChloeHoffman
4/20/15

Introduction
AnEPA(EnvironmentalProtectionAgency)inspectorperformedaroutineinspectionof
thechemistrystockroom.Duringtheinspection,he/shediscoveredanunknownchemicalandhas
givenusthreehourstoidentifytheunknownbeforeissuingafineforviolationoftheChemical
SpecificRightToKnowAct.Usethetimewiselytoinvestigatethechemicalsubstanceand
determineitsidentity.Therearetwelvepossiblechemicalsthattheunknowncouldbe.
Thepurposeofthisexperimentistodeterminetheidentityofanunknowncompound
usingtheskillsobtainedinpreviouslabsinthegeneralchemistrycourse.Inthisexperiment
differenttechniqueswillbeusedtoascertaintheidentityofanunknownsubstanceprovideby
thestockroom.ThedifferenttoolsthatmaybeusedinthisexperimentincludetheMeasureNet
spectrophotometer,MeasureNetpHprobeanddropcounter,theMeasureNettemperatureprobe,
andcalorimeters.
Differenttechniquesthatcouldbeusedtodiscovertheunknownsubstancecouldbea
solubilitytest,anelectricalconductivitytest,absorptionspectroscopy,emissionspectroscopy,
andtestingpHwiththepHprobe.Studentsshouldfirstperformasolubilitytestontheunknown
chemicalandadvancefromthatpointbasedonthetestresults.Makesuretowearsafetygoggles
atalltimesduringtheexperiment.Allsupplieswillbeavailableatthestockroom.

Experimental
PossibleChemicalstheUnknowncouldbe:
1. aluminum(s)
2. sodiumhydrogencarbonate(s)
3. bariumchloride(s)
4. ammonia(aq)
5. formicacid(aq)
6. sodiumhydroxide(s)
7. hydrochloricacid(aq)
8. iron(III)chloride(aq)
9. ethanol(
l
)
10. hexane(
l
)
11. urea(s)
12. potassiumsulfate(s)
ChemicalstobeusedtodetermineUnknown:
1.
2.
3.
4.
5.
6.
7.
8.
9.

0.1MHydrochloricacidsolution
pH4andpH7buffersolutions
0.1MSodiumhydroxidesolution
0.1MSilvernitratesolution
0.1MBariumchloridesolution
0.1MIron(III)nitratesolution
0.1MSodiumchloridesolution
0.1MPotassiumchloridesolution
Distilledwater

Tostartobtaintheunknownsubstancefromthestockroom.Testthesolubilityof
theunknownchemical.Dothisbyputtingasmallamountoftheunknownsubstancein
20mLofwater.Iftheunknownisasolidaddabout1gramandrecordtheexactamount.
Ifthesubstanceisaliquidaddapproximately1mLandrecordtheexactamount.Stirthe

substancewithastirringrodforaboutaminute.Ifthesubstanceisdissolvedthenitis
solubleifitdidnotdissolvethenitisinsoluble.Recordtheobservations.
Ifthesubstanceisinsolublethenproceedtoidentifythestateofthesubstance.If
thesubstancewassoluble,thenadvancetothenextparagraph.Ifthesubstanceisaliquid,
thanitisHexane.Thedensityofhexaneis.659g/mLtoconfirmthattheunknownis
hexanezeroagraduatedcylinderandputsomeoftheliquidinthecylinder.Makenoteof
theamountonthescaleandwhatnumberofmLthegraduatedcylinderreads.Plugthe
numbersintothisequation:
mass
Density= volume

Iftheinsolublesubstanceisasolidthenitisaluminum.Toconfirmthatthe
unknownisaluminumthedensityis2.70g/mL.Measureanamountoftheunknown
weighitandthenputitingraduatedcylinderwithwater.TakenoteofthechangeinmL
onthegraduatedcylinder.Calculatedensitywiththeequationabove.
Ifthesubstanceissolubleinwaterproceedtoperformanelectricalconductivity
test.Todothisyouwilltheconductivitydetectorwhichisacquiredatthestockroom.A
pictureoftheconductivitydetectorcanbeseenbelow.

Inplaceofthebeakersinthepictureseeninthepictureawatchglasswillbeused.Put

1520dropsofthesolutionmadewiththeunknowninawatchglass.Simultaneouslyimmerse
theconductivitydetectorelectrodesintothesolutioncreatedwiththeunknownonthewatch
glass.Ifthelightremainsoffthenthesolutionisnotanelectrolyte.Ifthelightisdimlylitthen
thesolutionisaweakelectrolyte.Ifthelightisbrightthesolutionisastrongelectrolyte.Record
observationsinlabreport.
IftheSolutionisaNonelectrolyte:
Ifthestateoftheunknownsubstancebeforeitwasmadeintoasolutionwasasolid.To
determinethefreezingpointofthesolutiontodothisathermogramwillneedtobeprepared.
Obtainatemperatureprobefromthestockroom.ToinitializetheMeasureNetstationpress
Main
Menu
,nextpress
F2Temperature
,then
F1Temperaturevs.Time
.Thenproceedtofilla
150mLbeakerwithiceandwater.Press
Calibrate
.Enter0.0thensubmergethetemperature
probeintheicewaterbath.Stirthetemperatureprobeuntilthetemperaturestabilizesnear0.
Pressthe
Enter
buttonandremovethetemperatureprobefromtheicewater.Toestablishscan
parameterspressthe
SetUp
buttonandpress
F1
.Usetheleftandrightarrowkeystoadjustthe
min
and
max
.The
min
temperatureshouldbesetbetween1518andthe
max
temperature
shouldbesetbetween7075.Setthe
min
fortheXaxisat0secondsandthe
max
at700
seconds.Press
Display
whentheparametersareset.Pourthepreparedsolutionintoa25x200
mmtesttube.Insertthetemperatureprobeandwirestirrerintothesolution.1.3cm.1.9cm.of
thetemperatureprobeshouldbecoveredbythesolution.Securethestopper.Usingaringstand

andclampsecurethetesttube,temperatureprobeandstirrerassemblyinsideanicebath.Theice
bathpreparetocalibratethetemperatureprobemaybeusedwiththeadditionofmoreicetokeep
thetemperaturenear0.Press
Start
ontheMeasureNetstationtobeginrecordinga
thermogram.Occasionallystirthesolutionuntilitfreezes.Whenthesolutionfreezes,press
Stop
ontheMeasureNetstationandsavethefile.Press
Display
toclearthescan.Removethetest
tubefromtheicebath.Discardofthefrozensolutioninthesink.Drythetesttubeand
temperatureprobe.Performasecondtrial.Thetemperatureprobedoesnotneedtobe
recalibrated.Outsideoflabpreparethethermogramsfromthesavedtabdelimitedfilesto
determinethesolutionsfreezingpoint.Ifthestateoftheunknownsubstancewasaliquidbefore
itwasdissolvedinwatertheidentityoftheunknownisethanol.Toconfirmthesubstances
identitydeterminethedensityofthesubstance.Ifthesubstancehasadensityofapproximately
0.789g/mLthesubstanceisethanol.Ifyoudonotknowhowtodeterminedensityreturnto
paragraph#2.
IftheSolutionisaWeakElectrolyte:
IfthesolutionisaweakelectrolytethenthesubstancewillbeeitherFormicAcidorAmmonia.
ThepHprobewillbeusedtodeterminethepHofthesubstance.First,calibratethepHprobe.To
dothisturnonthe
MeasureNet
stationandpress
MainMenu
.Thenpress
F2pHv.Volume.
In
thelistofchemicalsprovided,insertthepHprobeintothebuffersolutionwithapHof7.00.
Press
Calibrate.
Whenpromptedforthetemperatureofthebuffersolution,enterroom
temperature,thenpress
Enter
.
Enter
7.00whenaskedforthepHofthebuffer,thenpress
Enter
.
WhenthedisplayedpHvaluestabilizes,press
Enter
(pHvalueshouldbecloseto7.00,butit
doesnothavetobeexactly).
PressF1,
then
Display
toacceptallvalues.RemovetopHprobe

fromthebuffersolutionandrinseitwithdistilledwater.After,immersethepHprobeintothe
acidicorbasicsolution(makesuretoaddastirbarinsolution)thatisonamagneticstirrer.Turn
onthemagneticstirreronalowsettingandmakesurethepHprobedoesnotmakecontactwith
thestirrerintheunknownsolution.IfthetipofthepHprobeisnotcompletelyimmersed,add
morewateruntilitcoversthetip.IfthepHvaluedisplayedonthe
MeasureNetStation
isless
thanapHof7.00,thentheunknownisacidicandtheunknownsolutionisFormicAcid.Ifthe
pHvaluedisplayedonthe
MeasureNetStation
ismorethanapHof7.00,thenthesolutionis
basicandtheunknownisAmmonia.
IftheSolutionisaStrongElectrolyte:
Ifthesolutionisdeterminedtobeastrongelectrolytethenaflametestshouldbe
performed.Todothisobtainabunsenburnerandanichromewire.Turnonthebunsenburner.
Opentheairventsonthecollar.Rinsethenichromewirewithdistilledwaterwithabout3040
mLtoensurethattheirisnothingleftfrompreviousstudents.Afterthishasbeencompletedthe
bunsenburnermustbecleaned.Dothisbypouringasmallamountofdistilledwaterontoa
watchglass.Thenheatthenichromewireuntilitglowsbrightorange.Positionthewatchglass
neartheburnersairintake.Putthehotwireinthedistilledwaterandsplatteritintotheair
intake.Dumptheremainingdistilledwaterintothesin.Putapproximately1mLelectrolyte
solutionontothewatchglass.Repeatthesamestepsasdonewiththewater.Takenoteofthe
flamecolorandadvance.
Iftheflamecolorispurple,thentheunknownsolutioncouldbepotassiumsulfate.To
confirm,add1gramofBaCl2(s)tothealreadydilutedunknownandaprecipitatemustform.If

theflamecolorturnsgreen,thentheunknownsolutioncouldbeBariumChloride.Toconfirm,
add1gramofAgNO3(aq)totheunknownsolutionandaprecipitatemustform.IftheFlame
doesnotchangeanycolor,thenonecouldassumethattheunknownsolutionisHCl(proper
cautionandprotectionshouldbeusedwhenhandlingastrongacid).Toconfirmwhetherthe
unknownisHCla
MeasureNetStationpHprobe
canbeused(Seenextparagraph).Ifthe
Flamecolorturnsyellow,thentheunknownsolutioniseithersodiumhydroxideorsodium
hydrogencarbonate.TofindoutwhichoneapHprobewillbeused(Seenextparagraphfor
instructionswhensettingupthe
MeasureNet
pHprobe).
First,calibratethepHprobe.Todothisturnonthe
MeasureNet
stationandpress
Main
Menu
.Thenpress
F2pHv.Volume.
Inthelistofchemicalsprovided,insertthepHprobeinto
thebuffersolutionwithapHof7.00.Press
Calibrate.
Whenpromptedforthetemperatureof
thebuffersolution,enterroomtemperature,thenpress
Enter
.
Enter
7.00whenaskedforthepH
ofthebuffer,thenpress
Enter
.WhenthedisplayedpHvaluestabilizes,press
Enter
(pHvalue
shouldbecloseto7.00,butitdoesnothavetobeexactly).
PressF1,
then
Display
toacceptall
values.RemovetopHprobefromthebuffersolutionandrinseitwithdistilledwater.Insertthe
pHprobeintotheunknownsolutionsolution.IfthetipofthepHprobeisnotcompletely
immersed,addmorewateruntilitcoversthetip.IfthepHvaluedisplayedonthe
MeasureNet
Station
islessthanapHof10,thentheunknownisSodiumhydrogencarbonate.IfthepHis
over10,thentheunknownsolutioncouldbeSodiumHydroxide.Toconfirmthis,addFe(NO3)3
(aq).Aprecipitatemustform.

Results:Unknown#2
Wastheunknownchemicalsolubleorinsoluble?
TheunknownChemicalwasSoluble.
Unknownnumberofnonelectrolytecompound:#2

ElectricalConductivityTest:Unk#2

BrightnessofLight

Resultsnonelectrolyte

novisiblelightwhatsoever

Observationsofunknown:
Unknownisawhitesolid.Itlookslikeminisnowballsbutcanalsolooklikeacrushedwhite
powder.
Howdidyouconfirmtheidentityoftheunknown?
Toconfirmtheunknownafreezingpointdepressionwasperformed.
Freezingpointdepression,fortheunknown,nonelectrolytesolution
Trial1:
freezingpoint:1.734
Trial2:
freezingpoint:1.801
1.734+1.801
=1.75
2

T
=(Freezingpointofpuresolvent)(Freezingpointofsolution)
f

0(1.75)=1.75

1.75
m
1.86kgwater =0.941

Tf=Kf*
m

x
0.941
m
= .02

#ofmoles=.0188mol

1gurea
.0188moles

= 53.14 g/mole

IdentityofUnknown:
Urea
Discussion:
Hooray!Theunknownhasbeendeterminedwithinthetimeallottedandcannowbe
reportedtotheinspector.Theinspectorhasdecidedtonotissueafineandcannowcompletethe
restofhisinspection.Theunknownfoundinthebytheinspectorhasbeendeterminedtobe
Urea.Thisisclearbecausetheresultsofthesolubilitytestdeterminedthattheunknownwas
soluble.Thisisclearwhenthesoliddissolvedindistilledwatercompletely.Byfollowingthe
flowchartthenextexperimentperformedwastheelectricalconductivitytest.Tocompare
brightnessandknowforcertainwhethertheunknownisastrong,weakornonelectrolyteboth
wiresconnectingtothebatterywereputtogether.Aftertheyweresubmergedinthesolutionand
itwasmadesurethatthewiresdidnottouch.Thelightwasbarelyvisible,butwasdeterminedto
beanonelectrolyte,becauseeveniftheunknownsoliddissolvedindistilledwaterisa
nonelectrolyte,therearestillimpuritiesinthedistilledwaterused.Afterdeterminingthatthe
unknownwasanonelectrolyte,tobecertainafreezingpointdepressionwasperformedandafter

graphingtheresults,theconclusionwasclearandtheunknownwasUrea.Althoughthe
calculationsdeterminedwereslightlyoff,theresultswereaccurate,butnotasprecise.
Conclusion:
Todeterminetheidentityoftheunknownaseriesofexperimentswereperformed.Theresults
thatweredeterminetoldusthattheunknownwassoluble,anonelectrolytewhichwouldmean
theunknownsidentitywouldbeurea.Weconfirmedthisbyperformingafreezingdepression
andgraphingthedata,ourcalculationsweretheclosesttoUrea.Eachexperimentperformeddid
providethenecessarydatatoanswerthecentralquestion,whichwasforustodeterminethe
unknownfoundduringtheinspection.

Bibliography
Stanton,B.,Zhu,L.andAtwood,C.H.(2010).ExperimentsinGeneralChemistry:Featuring
MeasureNet:2ndEdition.Mason,Ohio:CengageLearning.
"Draft:ChemProposalFlowchart."
Gliffy
.1Apr.2014.Web.9Apr.2015.
<https://www.gliffy.com/publish/5557399/>.