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Experiment Report of Organic Chemistry 3
or ga")E#uen can be either pure "ub"tance" or mixture", eg pure pitch or a#coho#
0)
The mo"t po%erfu# component" ab"orbed by the ad"orbent %i## f#o% the
"#o%e"t -ie ./ and conver"e#y the #o%e"t ab"orbed fa"te"t f#o%" -ie */, %hi#e
the ab"orption of C i" bet%een . and *) The #onger the proce"" f#o% the greater
the di"tance bet%een the component and more perfect "eparation, but tae" a
#ong tube a" %e## a" the e#uent and ad"orbent that much)
Component" can be "eparated from other component" by pu"hing out and
cut ad"orbent ba"ed component") Each piece put into a "o#vent and fi#tered to
"eparate the ad"orbent, and the "o#ution %i## contain one component)
Component" can be "eparated from the "o#vent by deti#a"i techni$ue" or
recry"ta##i&ation)
THE KINDS OF CHROMATOGRAPHY
*a"ed on the type of e#uent and ad"orbent, chromatography can divided to
four %ay", name#y chromatography co#umn, paper, thin p#ate", and ga")
Column Chom!"o#!$h%
Chromatography co#umn chromatographic ad"orbent i" in"erted into the
tube -pipe/ g#a"") The ad"orbent "o#id" in po%der form, for examp#e a#umina,
after "eparation of each component contained in certain area" chromatography
preformance tube)
P!$& Chom!"o#!$h%
Paper chromatography i" a type of chromatography that u"e" paper a" an
ad"orbent and #i$uid a" e#uen) 3echanica# "eparation, the mixture of
component" dropped on paper -u"ed ad#ah paper chromatography/ %ith a "ma##
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pipette, for examp#e at t%o point" p and $ doe" not "et the paper i" hung "o that
"tab#e and in order e#uan #et ri"e "#o%#y, carrying component" terdapt at p dan$
ear#ier) Eventua##y it %i## be "een apart from one another component, becau"e
the difference in po%er ab"orbed in the paper)
Th'n L!%& Chom!"o#!$h%
Thin #ayer chromatography -TC/ u"ing a thin p#ate -"uch a" g#a"" or
meta# p#ate"/ %ere coated in "o#id" a" ad"orbent and dried) .fter the "#ab drop"
of the mixture to be "eparated and put into a ve""e# containing the e#uent, "uch
a" on paper romatogrfi)
G!( Chom!"o#!$h%
4a" chromatography i" ga" chromatography u"ing a" e#uennya, %hi#e thecomponent" in the app#iance %i## be converted into ga" and f#o% %ith the
e#uent) 5#o% ve#ocity component" %i## be different and #ead to the "eparation of
the component" %ith one another)
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'n a chromatographic techni$ue, the "amp#e i" a mixture of different ind"
of component" to be p#aced in the dynamic "ituation in the "y"tem con"i"ting of
the "tationary pha"e and the mobi#e pha"e) .## the chromatographic "eparation
depend" on the re#ative movement of each of the component" bet%een the t%o
pha"e") Compound" or component" that re"trained -inhibited/ i" %eaer by the
"tationary pha"e %i## move #ebihcepat of the component" are retained "tronger)
The difference bet%een the movement omponene %ith each other due to
difference" in the ad"orbent, partition, di""o#ution or evaporation bet%een the
t%o pha"e") 'f the"e difference" are big enough it %i## happen ppemi"ahanperfect#y) Therefore, in the "e#ection of the mobi#e pha"e chromatography and
the "tationary pha"e need" to be done in "uch a %ay that a## component" bia"ed
to move %ith different "peed" that can occur "eparation proce"")
Chromatography can be c#a""ified ba"ed on the type of pha"e" u"ed) 'n the
chromatographic mobi#e pha"e can be either ga" or #i$uid and the "tationary
pha"e can be either "o#id or #i$uid, then ba"ed on the moving!pha"e "tationary
pha"e, there are four ind" of "y"tem" romatogrfi, name#y6 ga"!#i$uid
chromatography, ga" chromatography!"o#id, #i$uid!"o#id chromatography and
#i$uid!#i$uid chromatography)
IR SPECTROSCOPY
'nfrared "pectro"copy -'( "pectro"copy/ i" the"pectro"copythat dea#" %ith
the infrared region of thee#ectromagnetic "pectrum, that i" #ight %ith a
#onger %ave#engthand #o%erfre$uencythan vi"ib#e #ight) 't cover" a range of
http://en.wikipedia.org/wiki/Spectroscopyhttp://en.wikipedia.org/wiki/Infraredhttp://en.wikipedia.org/wiki/Electromagnetic_spectrumhttp://en.wikipedia.org/wiki/Wavelengthhttp://en.wikipedia.org/wiki/Frequencyhttp://en.wikipedia.org/wiki/Visible_lighthttp://en.wikipedia.org/wiki/Spectroscopyhttp://en.wikipedia.org/wiki/Infraredhttp://en.wikipedia.org/wiki/Electromagnetic_spectrumhttp://en.wikipedia.org/wiki/Wavelengthhttp://en.wikipedia.org/wiki/Frequencyhttp://en.wikipedia.org/wiki/Visible_light -
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techni$ue", mo"t#y ba"ed onab"orption "pectro"copy) ." %ith a## "pectro"copic
techni$ue", it can be u"ed to identify and "tudychemica#") 5or a given "amp#e
%hich may be "o#id, #i$uid, or ga"eou", the method or techni$ue of infrared
"pectro"copy u"e" an in"trument ca##ed an 'n)!&* ($&+"om&"&-or
"pectrophotometer/ to produce an 'n)!&* ($&+"um) . ba"ic '( "pectrum i"
e""entia##y a graph of infrared #ight ab"orbance-or tran"mittance/ on the
vertica# axi" v") fre$uency or %ave#ength on the hori&onta# axi")
Typica# unit"of fre$uency u"ed in '( "pectra are reciproca#
centimeter"-"ometime" ca##ed %ave number"/, abbreviated a" cm71) 8nit" of '(
%ave#ength are common#y given in micron", abbreviated a" 9m, %hich are
re#ated to %ave number" in areciproca# %ay) . common #aboratory in"trument
that u"e" thi" techni$ue i" a 5ourier tran"form infrared -5T'(/ "pectrometer)
T%o!dimen"iona# '( i" a#"o po""ib#e a" di"cu""edbe#o%)
The infrared portion of the e#ectromagnetic "pectrum i" u"ua##y divided
into three region": the near!, mid! and far! infrared, named for their re#ation to
the vi"ib#e "pectrum)
The higher!energy near!'(, approximate#y 1000;000 cm71-0)
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are re"onant fre$uencie", i)e) the fre$uency of the ab"orbed radiation matche"
the tran"ition energy of the bond or group that vibrate") The energie" are
determined by the "hape of the mo#ecu#arpotentia# energy "urface",the ma""e"
of the atom", and the a""ociated vibronic coup#ing)
'n particu#ar, in the *orn;Oppenheimer and harmonic approximation", i)e)
%hen the mo#ecu#ar >ami#toniancorre"ponding to the e#ectronic ground
"tatecan be approximated by aharmonic o"ci##atorin the neighborhood of the
e$ui#ibriummo#ecu#ar geometry, the re"onant fre$uencie" are a""ociated %ith
the norma# mode"corre"ponding to the mo#ecu#ar e#ectronic ground "tate
potentia# energy "urface) The re"onant fre$uencie" are a#"o re#ated to the
"trength of the bond and thema"" of the atom"at either end of it) Thu", the
fre$uency of the vibration" are a""ociated %ith a particu#ar norma# mode of
motion and a particu#ar bond type)
Th& A,(o,"'on In)! R&*
-Figure6 too#" of '( "pectro"copy/
http://en.wikipedia.org/wiki/Resonant_frequencyhttp://en.wikipedia.org/wiki/Potential_energy_surfacehttp://en.wikipedia.org/wiki/Vibronic_couplinghttp://en.wikipedia.org/wiki/Born%E2%80%93Oppenheimer_approximationhttp://en.wikipedia.org/wiki/Molecular_Hamiltonianhttp://en.wikipedia.org/wiki/Ground_statehttp://en.wikipedia.org/wiki/Ground_statehttp://en.wikipedia.org/wiki/Quantum_harmonic_oscillatorhttp://en.wikipedia.org/wiki/Molecular_geometryhttp://en.wikipedia.org/wiki/Normal_modeshttp://en.wikipedia.org/wiki/Atomic_masshttp://en.wikipedia.org/wiki/Resonant_frequencyhttp://en.wikipedia.org/wiki/Potential_energy_surfacehttp://en.wikipedia.org/wiki/Vibronic_couplinghttp://en.wikipedia.org/wiki/Born%E2%80%93Oppenheimer_approximationhttp://en.wikipedia.org/wiki/Molecular_Hamiltonianhttp://en.wikipedia.org/wiki/Ground_statehttp://en.wikipedia.org/wiki/Ground_statehttp://en.wikipedia.org/wiki/Quantum_harmonic_oscillatorhttp://en.wikipedia.org/wiki/Molecular_geometryhttp://en.wikipedia.org/wiki/Normal_modeshttp://en.wikipedia.org/wiki/Atomic_mass -
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Fun#('on!l Gou$ A,(o,"'on $o('"'on In"&n+'"%
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C - H
Al!n&
?C>@, ?C>2? 2Aydrogen bond O> @0 ; @0 "
oub#e a""o"ia"ion O> @00 ; @200 ", #ebar
Carboxy#ic acid O> 2F00 ; 200 %
NH /Am'n& !n* !m'*&
#ou$ 1
.mine primer @00, @00 m
.mine "eunder @00!@@00 m
.mide primer @00,@00 m
>ydrogen bond @@0!@1 CO O ( 1200!11
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Saturated bond 1
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VI. TOOLS AND MATERIALS
Tool(:
! Capi##ary -1 item/
! 5i#ter paper -1 item/
! m# via# -1 item/
! Pipette -10 item"/
! 10 cm x 20 cm x 20 cm chamber -1 item/
! Spatu#a -1 item/
! 10 m# graduated cy#inder -1 item/
! 100 m# beaer g#a"" -1 item/
! Stir bar -1 item/
! 8D #amp -1 item/
! Set of in"trument" '( -1 item/
! Penci# 2* -1 item/
! T%ee&er" -1 item/
! Sma## g#a"" funne# -1 item/
M!"&'!l(:
! Samp#e
! i"ti##ate of methano#
! i"ti##ate of hexane
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! Ch#oroform
! cm x 20 cm TC p#ate
! 5ec#@reagent)
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VII. PROCEDURE
2.
!C#ean the practica# de" and e$uipment" for experiment
3. Chom!"o#!$h% T&("
Preparation of e$uipment"
(eady e$uipment"
1 mg Samp#e
.TC p#ate x
20 cm
!i#uted %ith
1m methano#
!4iven #ine upper
0,cm and #o%er
1,0cm
!4iven dot" on #o%er
#ine that ha" di"tance
0,cm
!Spotted "amp#e . on the dot" in
TC p#ate unti# it run" out
Spotted TC P#ate
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Spotted TC P#ate
!Put into chamber that fi##ed %ith
20m e#uent
!et the e#u"ion proce"" unti#
a#mo"t reached the upper #ine
TC P#ate
!Taen TC p#ate carefu##y, #et it dry
!Taen the "pot bond
!Put into fi#ter paper that ha" been "et
!Soaed %ith 1m methano#
!5i#trated
(e"idue 5i#trate
!Evaporated
!(ecry"ta#i&ed
Po%der of "amp#e
!'dentified by u"ing '(
Print out
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IX. ANALYSIS DATA
X. CONCLUSION
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REFERENCES
.n%ar, Chairi#, d) 1AA)Pengantar Praktikum Kimia Organik) Hogyaarta 653'P. 8niver"ita" 4ad=ah 3ada
Carey, 5ranci" .) 200B) Organic Chemistry Sixth Edition.Ne% Hor6 3cgra%!
hi##)
5e""enden (+) 5e""enden +S) 1AA1)Kimia Organic, Edisi ketiga ter=emahan .)
>arayana ud=aatrata, +i#id 1 dan 2) +aarta6 Penerbit Er#angga)
Said, 3oh, d) 1A
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ANS4ER 5UESTION
2. 4h!" '( "h& "&+hn'6u& o) &0"!+"'on7 (&$!!"'on !n* $u')'+!"'on o) !
+om$oun*8
An(9&:3echanica# extraction, "eparation and purification of a compound, the
three techni$ue" a## have the "ame princip#e of the "eparation of the
"ub"tance of the mixture into component" %ith each method
3. 4h!" '( ! +hom!"o#!$h'+ "&+hn'6u&8 9h% '( (&l&+"&* 'n "h&
$&$!!"'& TLC (&$!!"'on !,o&8
An(9&6
Chromatography i" u"ed to "eparate the "ub"tance of the mixture into it"
component") .## form" of chromatography %or ba"ed on thi" princip#e)
Chromatography i" a "eparation techni$ue ba"ed on the difference in
propagation "peed mixture component" in a particu#ar medium) 'n
chromatography, the component" to be "eparated bet%een t%o pha"e",
name#y the "tationary pha"e and the mobi#e pha"e) Stationary pha"e %hi#e
the mixture component" %i## %ith"tand the mobi#e pha"e %i## di""o#ve the
mixture component") Component" are ea"i#y retained on the "tationary
pha"e %i## be mi""ed) Khi#e the component" are "o#ub#e in the mobi#e
pha"e %i## move fa"ter) 8"ed preparative TC in order to obtain a "tab#e
$ua#ity of the "eparation of organic compound" in the "amp#e) 't i"
appropriate that the TC!P u"ed ab"orbent -"tationary pha"e/ %ith a
thicne"" of 0) to 2 mm of "i#ica ge# or a#uminum oxide and a #arge p#ate
-"i&e 20x20 cm and 20x0 cm/)
;. 4h!" '( "h& &lu&n" !n* 9h!" "%$& o) (ol&n" u(&* !( "h& &lu&n" !" "h&
"o$8An(9&:
The e#uent i" a mobi#e pha"e p#ay" an important ro#e in the proce"" of
e#ution for the feed "o#ution -feed/ to pa"" through the "tationary pha"e
-ad"orbent/) The type of "o#vent u"ed a" e#uent i" hexane, ch#oroform,
methano#)
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Purification i" done to "eparate the pure "ub"tance %ith dirt or po##ution
"ub"tance")
R&+%("!ll'=!"'on ,!('+ $'n+'$l&6 the cry"ta##i&ation proce"" begin" by
adding the compound to be purified %ith hot "o#vent unti# the "o#ubi#ity of
the compound at the #eve# of "uper!"aturated) 'n the"e circum"tance", if the
"o#ution i" coo#ed, the mo#ecu#e" of di""o#ved compound" %i## be "ticing
together, gro%" into cry"ta#" that %i## "ett#e at the bottom of the container)
Khi#e the dirt doe" not come precipitate di""o#ved)
5ormation of the cry"ta# it"e#f con"i"t" of t%o pha"e") Th& )'(" ("!#&i" the
primary nuc#eation or formation of the core, %hich i" the "tage %here the
cry"ta#" begin to gro% but do not "ett#e) Thi" "tage re$uire" a
"uper"aturated "tate of the "o#ute) Khen the "o#ution %a" coo#ed, the
"o#vent can not Lho#dL a## &a!"o#ute, re"u#ting mo#ecu#e" are "eparated from
the "o#vent "ticing together, and began to gro% into a cry"ta# nuc#eu") The
more core" are =oined, it %i## be the "ooner the cry"ta# gro%th)
Th& (&+on* ("!#&after the primary nuc#eation i" "econdary nuc#eation) .t
thi" "tage petumbuhan fa"ter cry"ta#, %hich i" characteri&ed by mutua#
attachment of the core" into "o#id cry"ta#")
>. 4h!" !& "h& )un+"'on( !n* ,&n&)'"( o) "h& "ool ? 'n("um&n" IR
($&+"om&"&8
An(9&:
E$uipment J '( "pectrophotometer in"trument i" a device u"ed to record
the infrared "pectrum trading and ea"y to u"e routine#y) 'nfrared
"pectrophotometry i" very important in modern chemi"try, %ho ma=or in
organic fie#d") Kere in"trumenta# in the di"covery of functiona# group", the
introduction of the compound mixture ana#y"i")
@. Th& &(ul"( o) "h& *!"! !n!l%('( !n* %ou '*&n"')'+!"'on7 +om$oun*
9h!" +!n %ou +h!#&8
An(9& :
/VITA INI AKU GA BISA NGERAKAN KARENA
BERHUBUNGAN SAMA PUNYAMU HASIL ANALISIS MU1
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ATTACHMENT