SEPARATION TECHNIQUES

Disusun oleh:
Sulfikar
Jurusan Kimia FMIPA UNM
SEPARATION TECHNIQUES
• To separate analyte from interferences, otherwise the interference may:
• generates an instrumental readout similar to the analyte, such that the
interference adds to the readout of the analyte, creating an error.
• suppresses the readout of the analyte e.g. by reacting with the analyte
Separation techniques
• There are many techniques for separating and concentrating the species of
interest.
• Such techniques exploiting differences in physico-chemical properties
between the various components of a mixture:
• molecular size, Mass or density
• Volatility, solubility,
• charge, shape and
• polarity
Classification of separation techniques
Basis of separation Separation techniques
Size Filtration
Dialysis
Size-exclusion chromatography
Mass or density Centrifugation
Complex formation Masking
Change in physical state Distillation
Sublimation
Recrystallization
Change in chemical state Precipitation
Electrodeposition
Volatilization
Partitioning between phase Extraction
Chromatography

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Separation based on size
(d)

a. Centrifugal filter b. Membrane c. Disposable d. Dialysis cassette

syringe filter filter manifold
e. size-exclusion chromatography

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ting_and_Preparing_Samples/7.6%3A_Classifying_Separation_Techniques
Separation based on mass or density
Components Centrifugal force Time (min)
(X g)
Eukaryotic cells 1000 5
Cell membranes, 4000 10
nuclei
Mitochondria, 15000 20
bacterial cells
Lysosomes, 30000 30
bacterial
membranes
Ribosomes 100000 180

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Separation by masking
Masking agent Elements whose ions can be
masked
CN- Ag, Au, Cd, Co, Cu, Fe, Hg, Mn,
Ni, Pd, Pt, Zn
SCN- Ag, Cd, Co, Cu, Fe, Ni, Pd, Pt, Zn
NH3 Ag, Co, Ni, Cu, Zn
F- Al, Co, Cr, Mg, Mn, Sn, Zn
S2O32- Au, Ce, Co, Cu, Fe, Hg, Mn, Pb,
Pd, Pt, Sb, Sn, Zn
Tartrate Al, Ba, Bi, Ca, Ce, Co, Cr, Cu, Fe,
Hg, Mn, Pb, Pd, Pt, Sb, Sn, Zn
Oxalate Al, Fe, Mg, Mn
Thioglycolic acid Cu, Fe, Sn
Changes in Physical State
(a) Simple distillation (b) Fractional distillation (c) Sublimation
Changes in Chemical state
For example: using a chemical reaction and a distillation to separate an
inorganic analyte from interferents
Analyte Treatment Isolated Species
CO32- CO32−(aq)+ 2H3O+(aq) → CO2(g) + CO2
3H2O(l)
NH4+ NH4+(aq) + OH−(aq) → NH3(g) + H2O(l) NH3
SO32− SO32−(aq) + 2H3O+(aq) → SO2(g) + SO2
3H2O(l)
S2− S2−(aq) + 2H3O+(aq) → H2S(g) + 2H2O(l) H2S

Another type of reaction is precipitation based on pH dependent solubility

Separation based on a partitioning between
phases
Techniques Phase system
Separation Techniques
• All separation techniques involve one or more chemical equilibria
• the degree of separation achieved can vary greatly according to
experimental conditions.
• To a large extent, attainment of optimum conditions has to be
approached empirically rather than by application of rigid theory.