Kul 1. Metoda Pemisahan

7/25/2019 Kul 1. Metoda Pemisahan

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Metoda PemisahanPendahuluan

Fithriani Armin, M.Si., Apt.


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What on Earth did scientist do before

Chromatography? Extraction is based on the diference in solubility material is grounded, placed with a solvent which dissolves soluble compounds. A second extract solvent . he mixture is placed in a

separatory !unnel "rystalli#ation also based on the diference o! solubility. he solubility is solved in a $xed volume o! solvent. he puri$ed compound crystalli#es as solution cools, evaporates or difuses

%istillilation

separates components based on their volatility typically via vapori#ation&condensation method

Filtration separate components o! a mixture based on their particle si#e. 'sed most o!ten to separate a li(uid !rom a solid

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Brief History of Chromatography)*+ - swett, a ussian botanist coined

the term chromatography. /e passedplant tissue extracts through a chal0column to separate pigments bydiferential adsorption chromatogrpahy

)*)1 .M 2illstatter, 3erman "hemist win4obel Pri#e !or similar experiement

)*55 6.S Palmer, American scientist usedswett7s techni(ues on various natural

products)*) ichard 8uhn used chromatography

to separate isomers oh polyene pigments9this is the $rst 0nown acceptance o!chromatographic methods

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Why Chromatography?

"hromatography is a very important

techni(ue in chemistry. he reason is that itcan separate one type o! molecules !romothers.


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"hromatography is an analytical techni(ueused to determine the purity o! a substance orto separate a mixture into its components.


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"hromatography is a non&destructiveprocedure !or resolving a complex mixture intoits individual !ractions or compounds.

his is a separation procedure and theseparated entities are identi$ed by otheranalytical techni(ues li0e 'nuclear magnetic resonance?, Massspectrometry etc. =n applications !or(uantitative analysis the measurement o! thearea under the curve in chromatogram is done.


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Denition & Principle inchromatography

Denition:

"hromatography is de$ned as the process o!separation o! the individual components o! amixture based on their relative a@nitiestowards stationary and mobile phases.


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he stationary phase re!ers to the solid orli(uid to which components in a mixture bindor adsorb.

he mobile phase re!ers to the li(uid or gasthat moves the components in a mixture over

the stationary phase.


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Menurut Farmakope Indonesia IV

Kromatografi adalah suatu teknik atau prosedurpemisahan zat terlarut oleh suatu proses migrasidiferensial dinamis dalam sistem yang terdiridari dua fase atau lebih yang salah satudiantaranya bergerak secara berkesinambungandalam arah tertentu dan didalamnya zat-zat itu

menunjukkan perbedaan mobilitas disebabkanadanya perbedaan dalam adsorpsi, partisi,kelarutan, tekanan uap, ukuran molekul ataukerapatan muatan ion.

2.


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Menurut IUPAC

Kromatografi adalah metode yang

digunakan untuk pemisahankomponen dalam sampel dimanakomponen itu terdistribusi dalam

dua fase yang salah satunya diamdan yang lainnya bergerak.


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Principle:he samples are subBected to Cow by mobile

li(uid phase onto or through the stablestationary phase. As in the de$nition theprinciple involved is separation o! !ractions o!mixture based on their relative a@nitytowards the two phases during their travel.

he !raction with greater a@nity to stationaryphase travels slower and shorter while thatwith less a@nity travels !aster and longer.


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"omponents in a mixture are separated basedon their diferent abilities to bind or adsorb tothe stationary phase, and on their diferentabilities to desorb or dissolve in the mobilephase.


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Types of Chromatography.

Dased on the mode or method employed inseparation chromatography is broadlyclassi$ed as

. !dsorption mode: /ere the stationaryphase is a solid while the mobile phase is

li(uid. he compounds travel on the stationaryphase under the inCuence o! mobile phasebased on their relative adsorption to the solidstationary phase.


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". Partition mode: =n this mode both thestationary and mobile phase are li(uids. Sothe compounds have a@nity based on theirpartition into the individual li(uid phases. heone with greater partition to stationary phasehas higher a@nity to stationary phase andvice versa.


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Dased on the nature o! stationary phase

it is o! two types:

a? #ormal phase chromatography: /ere the

stationary phase is polar in nature and hencethe compounds with higher polarity elute outlast while non polars come out $rst.


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b? %eerse phase chromatography:/ere thestationary phase is non&polar in nature andhence the compounds with lower polarityelute out last and vice&versa.

=n most /P6" analysis, the mode used is

reverse phase chromatography as many o!the biological, phytochemical compounds andeven drugs are polar in nature.


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Berdasarkan sifat fisika fase diam dan fase gerak


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Berdasarkan bentuk kemasan atau geometrik fasediam

Kromatografi planar, dimana fase diam tersebardalam bentuk lapis tipis pada lempeng kaca,

plastic atau aluminium (KLT) atau dalam bentuklembaran bahan selulosa (KK).

Kromatografi kolom, dimana fase diam dikemasdalam suatu kolom gelas atau logam (KG, KC,

dan KCSK).


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Berdasarkan mode pemisahan

* Adsorpsi : Kromatografi adsorpsi

* Partisi : Kromatografi Partisi

- Kromatografi fase terikat - Kromatografi pasangan ion

- Kromatografi penekanan ion

* Pertukaran ion : Kromatografi pertukaran ion

* Eksklusi ukuran : Kromatografi eksklusi ukuran

* Afinitas : Kromatografi afinitas


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Berdasarkan cara pengembangan / elusi

Pengembangan elusi (Elution Development)

Analisis frontal (Frontal Analysis)

Pengembangan pemindahan (DisplacementDevelopment) Pengusiran


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Advantages of chromatography

can separate very complex mixturesdrugs, plastics, flavorings, foods, pesticides,tissue extracts, fuels, air samples, watersamples, ...

very small sample sizes

separated components can be collected

individuallyanalyses can be highly accurate and precise


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Sheet chromatography

paper chromatography (PC)stationary phase is liquid soaked into a sheet orstrip of paper

mobile phase is a liquid solvent

some components spend more time in thestationary phase than others

components appear as separate spots spread outon the paper after drying or "developing"


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thin layer chromatography (TLC)stationary phase is a thin layer of adsorbent(Al2O3or SiO2, usually) coating a sheet of plastic

or glasssome components bond to the adsorbentstrongly; others, more weakly

as with paper chromatography, components

appear as spots on the sheet


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Column chromatography


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gas chromatography (GC)sample mixture is injected into a long tube (thecolumn)

mobile phase is an inert gas that sweeps the sample

down the tubestationary phase lining the tube selectively adsorbs ordissolves componentsthe stationary phase is a solid or very syrupy liquid

silicone polymers (like Silly Putty!) are often used asstationary phases in gas chromatographyadetectorresponds to separated components asthey leave the tube


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What is chromatography used for?

). $nding concentrations

gas chromatogram o! gasolineion chromatogram o! orange Buice


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each pea0 corresponds to a separatecomponent in the mixture

area o! each pea0 is proportional toconcentration


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2. chemical fingerprinting

species identification"killer" bees can be distinguished from nativebees by comparing gas chromatograms ofcuticle extracts

tracing contraband sources

detecting drugs in urine

Kul 1. Metoda Pemisahan

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