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WhatsintheContainer;aCapstoneExperiment

ColeAstin

WilliamReed

SamMilliner

LabSection#4

04/20/16

Abstract

We were asked to identify an unknown chemical compound within a three-hour


time span, with access to a small handful of known chemical agents and a number of
instruments. The unknown compound was one of twelve possible chemicals, and using a
sample of it, we were able to eliminate the options down to one possibility,thenpositively
identify itusingaseparateconfirmatorymethod.Thesamplegiven,labeled#13,turnedout
tobeurea,andwasidentifiedpositivelyusingafreezingpointdepressionanalysis.

Introduction

We need to identify an unknown and unlabeled substance in under three hours to


satisfy health and safety codes. We know it is one of thechemicalsonourchemicallist.We
have numerous methods we can use to identify the unknown chemical, including testing
pH, titration, electrolysis, testing the change in freezing points via colligative properties,
andobservationsofprecipitateformation.
This experiment needs to be performed because having an unknown substanceina
laboratory is a violation of the Chemical Specific Right-to-Know act. If we cannot indicate
conclusively what the chemical is, we will be issued a fine by the EPA. Furthermore, the
experiment is useful onthegroundsthatknowinghowtoidentifyanunmarkedchemicalin
safe and scientific ways is useful. Below is the list of possible chemicals that the unknown
couldhavebeen
Aluminum(s)
Sodiumhydrogencarbonate(s)
Bariumchloride(s)
Ammonia(aq)

Formicacid(aq)
Sodiumhydroxide(s)
Hydrochloricacid(aq)
Iron(III)chloride(aq)
Ethanol(l)
Hexane(l)
Urea(s)
Potassiumsulfate(s)

Experimental

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

EquipmentNeeded:
MeasureNetpHprobeanddropcounter
MeasureNettemperatureprobe
Conductivitydetector
Volumetricflasks
Labglassware
WatchGlass
9Voltbattery

Through observation the unknown was identified to be solid, white in color, and grainy in
texture with an unknown numberof13.Therewasnotapotentodorpresent.1.512gofthe
unknown was weighed in order to test for solubility and make an aqueous solution. The
unknown completely dissolved into 200mL of DI Water meaningitwascompletelysoluble.
ThiseliminatedAluminumasapossibilityaselementalaluminumisnotsolubleinwater.
Next the pH of the solution was tested using the MeasureNet pH probe. We
calibrated the pH probe using a buffer solution according to the pH calibration procedure.
The pH of our unknown was determined to be 7.2 which, being very close to 7,eliminated
sodiumhydroxideasapossibleunknown.
Then 20mL of unknownsolutionwasaddedtothreedifferentbeakers.SilverNitrate
was added to one beaker in a dropwise fashion for 15 drops and no precipitate formed
eliminating Barium Chloride as a possible unknown. Barium Chloride was added in a
dropwise fashion for15dropsandnoprecipitateformedeliminatingPotassiumSulfateasa
potentialunknown.Thethirdbeakerwasusedasareference.
With Aluminum, Sodium Hydroxide, Potassium Sulfate, and Barium Chloride
eliminatedthatleftSodiumHydrogenCarbonateorUreaasourpossibleunknown.An
electrical conductivity experiment was proposed and a small amount of tap water was
added to a watch glass. Next we dissolved approximately 1 gram of our unknown into the
approximately 5mL of water in the watch glass. Next a 9-volt battery with a positive wire
and a negative wire attached was used to test conductivity. The water solution conducted
very little to no electricity and it was concluded not tobeelectricallyconductiveenoughto
beSodiumHydrogenCarbonate.
Only Urea was left to positively identify so a freezing point depression experiment
was devised in order to test our solutions colligative properties. AhighconcentrationNaCl
solution was created in a 600mL beaker and had ice added to it in order to lower the
freezingtemperature.Next50mLoftheunkownsolutionwasaddedtoatesttubeaswellas
the MeasureNet thermometer and a metal mixing wire. A metal standwasusedtoholdthe
beaker in place, submerged in the salt water ice bath, and we began mixing the unknown
solution with the wire to lower its temperature more quickly. We continued this until the
unknown solution froze and recorded the data. We repeated this process for accuracy and
ourexperimentwasfinished.

Results(onseparatepagewithgraphs)

Discussion:
AfternarrowingthechemicaldowntoUrea,apositiveconfirmationwasneededtomake
surethatthechemicalwasindeedUrea.Afreezingpointdepressiontestwasusedto
determineiftheUreawasindeedtheunknownsubstance.UsingaVantHofffactorofone,
thetheoreticalwas T f =.2523C.Themeanexperimentalvaluecameouttobe
T f =.4756C.Whilethiswasconfusingatfirst,werecognizedwecanchangetheVantHoff
factorbasedourtheoreticalandexperimentalvalues.Usingtheequation
i=

T f Observed
T f predictednonelectrolyte

wewereabletodeterminethatitwasindeedUreabyusingthe

equation T f = K f m wheremismolality, K f is1.86and i istheVantHofffactor.By


plugginginour T f , i ,and K f ,wewereabletocomewithin7percentofouroriginal
weight(actualweight=1.51g,weightpredictedbyequation=1.63g)

ThisisinterestingbecauseUreaisanonelectrolytecompoundandshouldnotconduct
electricityandshouldhaveaVantHofffactorof1.Wespeculatethatthiscouldbecaused
bycontaminantsinourglasswarefrompreviousexperimentswhichwouldhavecausedthe
freezingdepressionpointtodecreaseevenfurther.Wecanruleoutthepossibilitythatwe
mayhaveerroneouslydisqualified N aHCO3 becausetheelectrolysistestgaveresultsfor
whatwouldhavebeenatmostaweakelectrolyte.Theprobesonthebatterycouldhavehad
contaminantsonitaswell,asitwasusedbytheentireclassandnotjustforour
experiment.

Weareconfidentinourresults.Wewereabletoeliminatealltheotherpossibilitiesand
makeapositiveidentificationofourunknownsubstancetowithin1/10thofagramofthe
measurementsweused.WeareperplexedwiththevantHofffactor,butwewerenotable
toidentifyanyothercompoundsthatwouldbeabletomatchupwithourresults.This
experimentcouldbeimprovedbycreatingastrongermolarsolutiontotest,whichwould
havegivenusstrongerresultsfromthestart.Athoroughcleaningofallofourtestbeakers
beforehandcouldalsohelpwithavoidinganycontaminants.Besidesthat,wefeelthatour
experimentworkedthewayweplannedandwearehappywithourresults.

Conclusions

Based on our calculations, and the stepsweperformedinourFlowChartandexperimental


procedure, weareconfidentthattheunknowncompound,markedas#13,isurea.Although
there couldhavecertainlybeenbettermethodsofidentificationthatwedidnothaveaccess
to,whatwemanagedshouldsufficeforacompleteidentificationwithoutanyrealdoubts.
Bibliography

Stanton, B., Zhu, L., & Atwood, C. H. (n.d.). General Chemistry Lab Manual: Chem 1215 and
Chem1225.

V.K.VENKATESANANDC.V.SURYANARAY,CONDUCTANCEANDOTHERPHYSICAL
PROPERTIESOFUREASOLUTIONS;Physico-ChemicalLaboratory,AnnamlaiUniversity,
SouthIndia