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Functional Group Analysis:

Hydroxyl group (-OH)


Alcohol
Phenolic
X gm of alcohol contain 17 gm of hydroxyl group

3 methods
a. Acetylation
b. Phthalation
c. Oxidation with periodates (periodic acid for polyhydroxy compounds)

a. Acetylation: R(OH)n where n is no. of hydroxyl group.


R(OH)n + (CH3CO)2O → R-O-COCH3 (Ester) + n CH3COOH (acetic acid)
Acetic acid is titrated against standard NaOH

Pyridine is used as neutral solvent due to following factors:


 Inactive towards the reagent
 Remove the acid produced by salt formation
 Serves as a catalyst
R-OH + (CH3CO)2O → R-O-COCH3 + (C55NH)+ (CH3COO)-
(pyridinium acetate)
Acetylation reagent:
Acetic anhydride + pyridine
1 part 3 part

Preserved with a guard tube containing Na-CaCl2

NaOH solution is alcoholic.


Procedure:
(Material) + Acetic anhydride + few drops of pyridine → Reflux for 45 min + water
(converts excess of Ac2O to Acetic acid). Titrate with std. NaOH. Take one blank

Mixed Indicator:
0.1% cresol red + 0.1% thymol blue Neutralised with NaOH
1 part 3 part
Color change: pH 9.8

Calculations:
W = wt (g) of sample
V1= Vol. (ml) of NaOH ( Blank)
V2= Vol. (ml) of NaOH ( sample)
N= Normality of NaOH solution

% of hydroxyl gr : {(V1-V2) x N} / 100 x (17/ w) x 100

1000 ml of N NaOH ≡ 1-Oh group


1000 ml of N NaOH ≡ 17 gm ,, ,,
(V1-V2) 1000 ml of N NaOH ≡ {(V1-V2) x 17 x N} / 1000 gm of –OH gr.
Now, w gm contain {(V1-V2) x 17 x N} / 1000
100 gm contains (V1-V2) x 17 x N x 100
……………………………………….
1000 x w

Use of Blank Titration:


Blank gives absolute concentration of reagent. Unavailable losses of the chemicals
by glass or cork etc. will be compensated. The chemical loss will be identical.