Chemical Impurity

CHEMICAL IMPURITIES

Chemical Impurity to be analysed

Procedure for analysis

Reaction expected

MPL

Inference

1. Ammonia

10 ml of sample in a test tube, add few drops of Nessler’s reagent 

Deep yellow or brown or black precipitate

0.06 ppm

Ammonia

2. Chloride

10ml of sample in a test tube, add a few drops of silver nitrate

White precipitate

250 ppm

Chloride

3. Sulphate

10 ml of sample add a few drops of HCl and a few drops of Barium Chloride

White precipitate formation hastened by heat

250 ppm

Sulphate

4. Nitrites

10 ml of sample, add a few drops of sulphanilic acid and add few drops of a -naphthalamine. Shake well.

Formation of pink colour

Not even

5.Nitrates                 
   (If nitrites are
    absent)

10 ml of sample , add a few drops of sulphanilic acid, add few drops of a -naphthalamine and pinch of Zinc dust

After 3 minutes a pink colour is noticed

1.5 ppm

Nitrates

6. Nitrates                 
     (If nitrites are
     present)

5ml of sample add equal quantity of brucine solution. Effervescence settles down run con. H 2 SO 4 along the sides agitate gently.

Formation of pink colour 

1.5 ppm

7. Phosphate

10 ml of sample, add a few drops of  ammonium molybdate solution.  Warm and agitate gently

Yellow precipitate soluble in ammonia solution and reappears

Not even in traces

Phosphate

8. Fluoride

10 ml of sample add a few drops of Ferric chloride

formation of White crystalline precipitate 

1 ppm

Fluoride

9. Cyanide

10 ml of sample add a few drops of ferrous sulphate, boil add HCl to obtain clear solution, add few drops of FeCl 2

A greenish to blue colour  is developed

Not even in traces

Cyanide

   

Last modified: Wednesday, 9 March 2011, 11:30 AM