Suraj Sir Chemistry
surajsirchem.live ›
Purification of Organic Compounds · JEE Advanced

Separation Techniques

Every method anchored to the one physical property it exploits — with a live diagram for each. Volatility, solubility, adsorption affinity, or travelling with steam.

TechniqueProperty exploitedTypical situation
SublimationSolid → vapour directlySublimable solid + non-sublimable one
CrystallisationSolubility varies with temperatureSoluble hot, sparingly soluble cold
Simple distillationLarge boiling-point gapVolatile liquid + non-volatile / far-boiling
Fractional distillationSmall boiling-point gapTwo miscible, close-boiling liquids
Steam distillationVolatile in steam, water-immiscibleDecomposes near its own b.p.
Reduced-pressure distn.b.p. falls as pressure fallsHigh-boiling / heat-sensitive liquid
Differential extractionUnequal solubility in two solventsCompound in water → organic solvent
ChromatographyDifferential adsorption / partitionSmall amounts, very similar components

01Sublimation

Principle. Some solids pass straight from solid to vapour on heating and re-solidify on cooling, without melting. Gentle heat drives the pure compound off as vapour, which re-deposits as a sublimate on a cool surface, leaving the non-sublimable impurity behind.

cotton plug puresublimate impure solid gentle heat
Fig 1 · Pure vapour deposits on the cool inverted funnel; the non-volatile impurity stays in the dish.

Applies to camphor, naphthalene, anthracene, benzoic acid, ammonium chloride and iodine — freed from non-sublimable impurities such as NaCl or sand.

02Crystallisation

Principle. A solid dissolves far more in hot solvent than cold. Dissolve the impure solid in the minimum hot solvent to saturate; on cooling the pure compound — less soluble cold — crystallises out, while soluble impurities stay in the mother liquor and are filtered off.

hot saturated solution → cool pure crystals form; impurities stay dissolved
Fig 2 · On cooling, the pure compound crystallises; charcoal can be boiled in first to adsorb coloured impurities.
Fractional crystallisation

Two solids of different solubility: repeated, controlled cooling makes the less-soluble one crystallise first. Separate and re-crystallise each crop — the classic route to KClO₃ from KCl.

03Distillation — the four variants

Principle. Separation by boiling point. Heat the mixture; the more volatile component vaporises, passes to the condenser and is collected as the distillate, while the less-volatile material stays in the flask.

(a) Simple distillation

For a large boiling-point gap (≈ 25 K or more), or a volatile liquid from a non-volatile solid — e.g. chloroform (61 °C) from aniline (184 °C), or water from salt water.

thermometerLiebig condenser water outwater in distillateheat
Fig 3 · The thermometer bulb sits at the side-arm to read vapour temperature; vapour condenses and drips into the receiver.

(b) Fractional distillation

For close boiling points. A fractionating column gives many vaporisation–condensation cycles, each enriching the vapour in the more volatile component. Basis of petroleum refining and of separating acetone (56 °C) from methanol (65 °C).

thermometer fractionatingcolumn Liebig condenser water outwater in low-boiling fractionheat
Fig 4 · The packed column provides many equilibrium stages, sharpening the separation of close-boiling liquids.

(c) Steam distillation

For liquids that are steam-volatile, immiscible with water, and decompose near their b.p. Compound and water each add their own vapour pressure, so the mixture boils when the total reaches atmospheric — below 100 °C.

ptotal = pwater + pcompound
condenser water outwater in distillate steam generatormixture flask
Fig 5 · Steam carries the volatile compound over; the distillate is compound + water, easily separated afterwards.
JEE favourite · o- vs p-nitrophenol

o-Nitrophenol has intramolecular H-bonding (chelation) → not associated → steam-volatile, distils over.

p-Nitrophenol has intermolecular H-bonding → highly associated → not steam-volatile → stays behind. (Same logic gives ortho the lower boiling point.)

(d) Distillation under reduced pressure

A vacuum pump lowers the pressure above the liquid, which lowers the boiling point. High-boiling or heat-sensitive liquids then distil well below their decomposition temperature — used for glycerol and to concentrate sugarcane juice.

thermometercondenser water outwater in distillate to vacuum pump gentle heat
Fig 6 · Connecting the receiver to a vacuum pump drops the boiling point, protecting heat-sensitive compounds.

04Differential (solvent) extraction

Principle. A compound in water is shaken with an immiscible organic solvent in which it is more soluble. It distributes between the two layers by the distribution (partition) law:

KD = (conc. in organic solvent) / (conc. in water)
organic layer(solute-rich) aqueous layer stopcock run lower layer off first
Fig 7 · The two immiscible layers settle; the lower layer is drained through the stopcock and each is collected separately.
Why many small extractions beat one big one

For a fixed total solvent volume, several small portions remove more compound than one large portion — each fresh portion re-establishes the KD equilibrium and pulls across more solute.

05Chromatography

Principle. Components separate by their differing affinity for a fixed stationary phase vs a moving mobile phase. Strongly-held components move slowly; those preferring the mobile phase move fast — so the mixture spreads into separate zones. Uniquely powerful for small amounts of very similar substances.

Column chromatography (adsorption)

The mixture is loaded on an adsorbent-packed column (silica / alumina) and washed down (eluted) with solvent. The least-adsorbed component moves fastest and emerges first; fractions are collected separately.

eluent in least adsorbed most adsorbed collect
Fig 8 · Bands travel down at different rates and leave the column as successive fractions.

Thin-layer chromatography (TLC)

The mixture is spotted near the base of an adsorbent-coated plate; solvent rises by capillary action, carrying components to different heights. Each is characterised by its retardation factor:

Rf = (distance moved by component) / (distance moved by solvent front)
solvent front baseline (spots applied) high Rf low Rf
Fig 9 · A more strongly-adsorbed component travels less → smaller Rf; one more soluble in the mobile phase travels further → larger Rf.
Reading Rf correctly

More strongly adsorbed → travels less → smaller Rf. More soluble in the mobile phase → travels further → larger Rf. Always 0 < Rf < 1, and fixed for a compound under set conditions — so it identifies components.

Paper chromatography works by partition: the stationary phase is water held in the paper, and components partition between it and the moving solvent — the same KD idea as extraction. Widely used for amino acids and sugars.

06Master comparison

MethodBasisBest example
SublimationSolid → vapour → solidCamphor, naphthalene, NH₄Cl, I₂
CrystallisationSolubility hot vs coldBenzoic acid, sugar, alum
Fractional crystln.Two solids, different solubilityKClO₃ from KCl
Simple distn.Large b.p. gapChloroform (61) from aniline (184)
Fractional distn.Small b.p. gapCrude oil; acetone / methanol
Steam distn.Steam-volatile, water-immiscibleAniline; o-nitrophenol; oils
Reduced-pressure distn.Lower pressure → lower b.p.Glycerol; sugarcane juice
Differential extractionPartition (KD)Compound from water into ether
Column / TLCDifferential adsorptionReaction mixtures; dyes
Paper chromatographyDifferential partitionAmino acids, sugars

07JEE Advanced traps

IG @suraj.thechemistWeb surajsirchem.live Email info@surajsirchem.liveCall +91 84259 53496