LabReport

G
r
o
u
p

m
e
m
b
e
r
s
:
1. Pichayatida
2. Thanatcha
3. Katechaya
4. Panaporn
5. Patsatorn

Srisakulpinyo
Thanapaisan
Thongdang
Wanthayawat
Yorkchaiyapruk

1109#5
1109#14
1109#15
1109#18
1109#20

Introduction:
Oneofthemostimporatantthingsinchemistryistoknowhoweach
substancecombiningtogethertoformacompound.Compoundsarethepure
substanceswhicharemadefromtwoormoreelementscombinedinafix
composition.When2ormoreelementscombined,thenewcompoundarecreated.
Butbeforethenewcompoundiscompletelyformed,thereweremanyprocesses
happenedwhenthecompoundareformedsuchasprocessoffiltrationand
crystalization.Furthermore,
filtrationistheprocessofseparatingsolidmatterfroma

liquid,bylettingthesmallerparticlestopassthrough,calledafilter.Theliquidwhich
haspassedthroughthefilteriscalledthefiltrate.Thefiltermaybepaper,cloth,
sand,orotherporousmaterial.Crystalizationisawaytopurifyingthecompoundby
addingahotsolventinthesolutiontocompletelydissovedthesolute.Aswhenit
cools,crystalareformed.

Objective:
Thepurposeofthisexperimentistoformthecombiningsubstancenamed
TetramethylammoniumiodineandIodinetosynthesizingthenewcompound
namedTetramethylammoniumpentaiodidebydissolvingwithEthanol.This
experimentalsodemonstratestheprocessofcrystalizationandfiltration.

Synthesisoftetramethylammoniumpentaiodide
Me4N+I+2I2>Me4N+I5

Procedure:
1.Addtoa50mLbeakertetramethylammoniumiodide(0.5g).Useastirringrodto
breakupclumpsofMe4N+I.
2.Addiodine(1.3g)and95%ethanol(12mL).
3.Inafumehood,gentlyheatthebeaker,withstirring,onahotplateforabout10
minutesuntiltetramethylammoniumiodidehasdissolved.

4.Heatatalowtemperaturetopreventprematurecrystallization.
5.Removefromtheheatandallowthebeakertocoolundisturbed.(Agitatingthe
solutioncancausesmallercrystalstofromwhicharemoredifficulttoisolateand
tendtooccludeimpurities)
6.Thecrystalsshouldformduringthistime.
7.Onceatroomtemperature,furthercoolingcanbeachievedbyplacingthebeaker
inanicebathforabout10minutes.Onlyputthesolutiononiceifnecessary.During
thistime,setuptheapparatusforsuctionfiltration.
8.Usingvacuumfiltration,collectthecrystalsandwashthemwithhexanes(5mL
portionsuntilfiltratedroppingfromfunneliscolorless,max.5washings).
9.Airdrytheproductwithweigh.
10.Handinasample,inacappedvial,labelledwithyourname,thenameofthe
compoundandthedatetothelabinstructor.

Materials:
Gloves
Tube
Beaker
Flask
Sterringglass
Goggles
Iodine

Labcoat
Filterpaper
Vacuumfiltration
Ethanol
Tetramethylammoniumiodine
Weigningapparatus
Watchglass

Data:
Beforecrystallization

Aftercrystallization

Tetramethylamoniumiodine0.5g
Iodine0.59g
Ethanol12ml

Me
N
I
of0.76g
4
5

Smallcrystal

DiscussionQuestions:
Calculatenumberofmoleofeachcompound.

MassofMe=15.0345g1.0023mol
MassofI=126.90447g1mol
MassofN=14.00674g1mol
tetramethylammoniumiodide(0.5g)/Me4N+I
0.5/201.04921=0.0024mol


Calculatepercentyield.
(actualyield/theoriticalyield*100)

1.62g/1.77gx100=91.53%

Whydoweusevacuumfiltrationnotgravityfiltration?

Weusevaccumfiltrationtofilteringthecrystalbecausethisvacuumfiltrationhave
lesspressurecomparingtothegravityfiltration.Usingthevacuumfiltrationwouldget
theresultfasteranditfiltratethoroughlybetter.

tetramethylamoniumiodine0.5g
iodine0.59g
ethanol12ml
Then,wecoolitwithice
Crystalizationformcrystalveryhard
Outcomesmallcrystal
Outcome0.76g

Analyzingresults:
Inthisexperiment,wesynthesizedtetramethylammoniumpentaiodideby
usingTetramethylammoniumiodideof0.5gandiodine0.59g.Then,wecombined
thesetwosubstanceswithethanolof12ml.Weheatedupthesesubstanceuntil
thecrystalizationprocesshappen.Afterwegotthecrystals,weneedtowashedthe
crystalswithhexaneandfilteritwiththevacuumfiltration.
Intheexperiment,wewaitedforthecrystaltobeformedforalongtime
becauseweusedthelessamountofiodine.Itmeanedthatlessamountofiodine
effecttheratewhencrystalwereformed.Theamountofiodinebeingusedinthe
experimentalsodeterminedthesizeofthecrystal.Accordingtotheamountwehave
used,itmakeasmallercrystal.Thecrystalwehadwaspurpleandbrownishcolor.
Although,wehavebeensuccessfulinourexperimentbutwehadsome
difficultiesduringtheexperiment.Thedifficuliesarethatthecrystalwerehardto
formedduetotheamountofiodineweused.Wehadtocoolitwithicetomakethe
crystalformedclearer.

Conclusion:
Accordingtothisexperimentourgroupusemanysubstancetoformthe
cystal.Forexample,tetramethylammoniumiodide,iodine,ethanolandhexanesto
runtheprocess.Soweknowthewayhowtocalculatethemoleofeachcompound
andbringittocalculatethepercentyield.Thisexperimenthelpsusknowthatactual

yieldandtheoriticalyeildarerelatetoeachother.Moreover,weknowtheprocess
howtoformthecrystalizationbyusingthesynthesisoftetramethylammonium
pentaiodide.

Picturesfromtheexperiment:


References:

Crystalization.(n.d.).Retrievedfrom
http://orgchem.colorado.edu/Technique/Procedures/Crystallization/Crystallization.ht
ml

Filtration.(2009).Retrievedfromhttp://www.lenntech.com/chemistry/filtration.htm