experiment fix klt.doc

8/10/2019 Experiment fix KLT.doc

1/18


2/18

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##


3/18


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)


4/18


'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


5/18


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)


6/18


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


7/18


Fun#('on!l Gou$ A,(o,"'on $o('"'on In"&n+'"%


8/18


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


9/18


Saturated bond 1


10/18


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


11/18


! Ch#oroform

! cm x 20 cm TC p#ate

! 5ec#@reagent)


12/18


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


13/18


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


14/18


IX. ANALYSIS DATA

X. CONCLUSION


15/18


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


16/18


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#)


17/18


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


18/18


ATTACHMENT

experiment fix klt.doc

Documents