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Methode
1
Metode Isolasi dan Pemurnian
Extraction
Recrystallization
Melting and Boiling Points
Distillation
Sublimation
Chromatography
2
Extraction
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Extraction
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Separatory Funnel
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Distribution Coefficient
Defined as
concentration of solute in solvent A
Kd = concentration of solute in solvent B
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Multiple Extractions
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Recrystallization
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Solvent Properties
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Melting and Boiling Points
Melting Point
Solids finite vapor pressure
As T increases the vapor pressure increases
At the mp solid and liquid are at equilibrium
vapor
melting
solid liquid
freezing
10
Melting Points
Physical characteristic
Generally reproducible
Presence of trace impurities depresses mp
Pure compounds melt over 0.5 to 2 degrees
Impure compounds have larger ranges
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Boiling Points
12
Boiling Points
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Distillation
moles A
mole fraction A =
moles A + moles B
Simple
Fractional
Vacuum
Steam
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Simple Distillation
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Fractional Distillation
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Which?
Simple Fractional
Simple setup Complicated setup
Fast process Slow process
Consumes less E Energy intensive
Poorer separation Better separation
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Azeotropes
Constant boiling liquid mixtures
Cannot be purified further by distillation
95.6% EtOH + 4.4% HOH: bp = 78.2 o
Vapor composition is the same as the liquid
composition
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Vacuum Distillation
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Vacuum Distillation
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Vacuum Pump
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Steam Distillation
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Sublimation
Evaporation generally requires melting
Some substances evaporate from solid state
Sublimation
Iodine, carbon dioxide
High vapor pressures below mp
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Purification by Sublimation
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Sublimation
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Chromatography
Thin-Layer (TLC)
Gas-Liquid (GC)
Liquid (LC)
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Chromatography
29
TLC
Stationary phase
glass or plastic plates coated with thin layer of
adsorbent
Silica gel, alumina, cellulose
Mobile phase
Solvent or mixture of solvents
Determined by sample polarity
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Gas-Liquid Chromatography
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GC
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Process
Sample is injected
Heated injection port
Vaporized into gas
Components are partitioned between gas and
stationary phase
Equilibrium depends upon
Temperature, gas flow rate, solubility in stationary
phase
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35
Column
Packed Columns
Interior diameter = 2 4 mm
Length = 2 3 m
Coating = 0.05 1 micrometer
Capillary Columns
Interior diameter = 0.25 0.5 mm
Length = 10 100 m
Coating = 0.1 5 micrometer
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Stationary Phase
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Detectors
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Thermal Conductivity
Heat loss is related to gas composition
Hot filament generates electrical signal
Constant in flow of He gas
Sample causes change in electrical signal
40
Flame Ionization
More sensitive
Non-flammable samples are not detected
Carrier gas is mixed with hydrogen
Sample is burned producing ions
These alter electrical output generating a signal
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FID
42
Liquid Chromatography
Column
Flash
High Performance
Separate mixtures of low volatility
Useful for nanogram to multi gram quantities
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Column Chromatography
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Flash Chromatography
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HPLC
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HPLC Detectors
UV Detectors
Fixed wavelength
Multi-wavelength
Diode Array
Electrochemical conductivity
Fluorescence
Refractive index
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Refractive Index
Bulk property
Changes in Rf by solute in the eluent
Developed in 1942
Limited sensitivity
Useful for compounds that
Do not fluoresce
Do not absorb uv
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Rf Schematic
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Fluorescence
Light is emitted by molecule excited by
electromagnetic radiation
Photoluminescence
Release of light stops on removal of source
Release of light is immediate
Fluorescent
Release is delayed
Release continues after removal of source
Phosphorescent
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Fluorescence
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Schematic
56
UV Detectors
Compounds respond to light in 180 350 nm
Contains pi electrons, lone pairs of electrons,
carbonyls, etc.
Very sensitive
Relationship based upon Beers Law
Fixed single wavelength lamp; Hg at 254nm
Inexpensive
Somewhat sensitive
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Schematic of Fixed Wavelength
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UV Detectors
Multi-wavelength Detector
Light source releases light over a range of
wavelengths
Deuterium or Xenon lamps are used
Dispersion and diode array
Dispersion detectors are almost not sold
Diode array is most common
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Dispersion UV Detectors
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Schematic of Dispersive Cell
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Diode Array
Deuterium lamp
Light from all wavelengths is passed through
the cell and dispersed over an array of diodes
Light is continuously monitored by all diodes
Fluorescence is still a concern
Output from any diode may be looked at
Sensitivity is a little less than fixed wavelength
More than adequate
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Schematic of Diode Array
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