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ELEMENTAL ANALYSIS

EXPERIMENT OBSERVATION INFERENCE PRINCIPLE AND REACTIONS

TEST FOR NITROGEN

1 ml SFE + 0.1g Ferrous sulphate Prussian blue precipitate or Nitrogen present Ferrous sulphate Sodium Ferrocyanide
crystals. Heat to boiling and add 2 drops Bluish green colour Sodium ferrocyanide combines with ferric ions which are produced by air
of conc. H2SO4 carefully. oxidation in the alkaline solution to give insoluble Prussian blue
precipitate (ferric ferrocyanide). Ferrous and ferric hydroxides also
precipitate but dissolve on acidification with sulphuric acid.

Prussian Blue
TEST FOR SULPHUR
a) 1 ml SFE + 1ml dilute Acetic acid Black precipitate Sulphur present
solution + 2 drops Lead acetate solution.

b) 1 ml SFE + Sodium nitroprusside Violet or purple colour Sulphur present


solution

TEST FOR HALOGENS


a) White precipitate easily soluble in Chlorine present
a) 1ml SFE + 2ml dil.HNO3 boil for 2 Ammonium Hydroxide
min. Cool and add Silver nitrate
solution. b) Pale yellow precipitate sparingly Bromine present
soluble in Ammonium Hydroxide
NOTE: If Nitrogen and or Sulphur are
absent, boiling is not necessary. c) Yellow precipitate insoluble in Iodine present
Ammonium Hydroxide
If nitrogen and/or sulphur are present, the addition of silver nitrate will precipitate
white silver cyanide and/or silver sulphide in addition to the silver halides.
Therefore, boiling after addition of nitric acid is necessary. Nitric acid liberates
volatile HCN and/or H2S which are driven off during boiling.

b)1ml SFE + 1ml dil.H2SO4 + 1ml a) Colourless globule Chlorine present


Carbon tetrachloride + chlorine water
added dropwise with vigorous shaking b) Brown or reddish globule Bromine present

c) Violet globule Iodine present


PRELIMINARY EXAMINATION

EXPERIMENT
EXPERIMENT OBSERVATION
OBSERVATION INFERENCE
INFERENCE REACTIONS REACTIONS

PHYSICAL STATE Solid Amides, Anilides,


Carbohydrates, acids

LIquid Alcohols, Aldehydes,


Ketones, Phenols, Amines

COLOUR Yellow Nitro compounds,


Benzaldehyde

Brownish to Pink Amines, Phenols

Colourless Acids, carbohydrates,


Amides
Pleasant Alcohols, Hydrocarbons

ODOUR Phenolic Phenols

Fishy Amines

Fruity Esters

Bitter Almonds Benzaldehyde, Nitrobenzene


IGNITION TEST

Ignite a small amount of Sooty flame Aromatic compound


compound on a spatula by
keeping it in flame of Bunsen No Sooty flame Aliphatic compound
burner.
No Soot, white residue Urea

Charred, froth residue Carbohydrates


TESTS FOR
UNSATURATION
Organic compounds containing > C = C < and / or —
Bromine Test C = C – bonds are called unsaturated compounds.
Addition of bromine to an alkene results in the
Sample dissolved in 2ml CCl4 + Decolorisation of bromine Unsaturated compound formation of vicinal dibromide. The reddish orange
Bromine solution in CCl4 solution without evolution of HBr colour of the solution of bromine in carbon
dropwise tetrachloride disappears on reaction with an alkene

Decolorisation of bromine Highly reactive aromatic Phenols and aromatic amines react by substitution
solution with evolution of HBr compound (Phenols, reaction with bromine and an equivalent quantity of
aromatic amines etc) HBr is evolved.
No Decolorisation Saturated compound

Bayer’s Test Alkenes decolorize the neutral/alkaline KMnO4


Sample dissolved in 2ml water or Pink color is discharged Unsaturated compound solution and vicinal glycols are formed.
Acetone or ethanol + 2% KMnO4
solution dropwise Pink color is not discharged Saturated compound
SOLUBILITY TEST

Procedure: In a dry test tube take 100mg of the solid sample or 0.2ml of the liquid sample and add successively 1ml portions of the solvent shaking
vigorously until 3ml has been added. If the sample does not dissolve completely in 3ml of the solvent it may be regarded as insoluble in that solvent.

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