Pharmaceutical Analysis/Gravimetry

DETERMINATION OF NICKEL AS THE DIMETHYLGLYOXIMATE:

Discussion: Nickel is precipitated by the addition of an ethanolic solution of
dimethylglyoxime, i.e.H2 DMG to a hot, faintly acidic solution of nickel salt and then
adding a slight excess of aqueous ammonia solution (free from carbonate).The precipitate
is washed with cold water and then weighted as nickel] dimethylgyoximate after drying
at 110-120C.
Ni2+ + 2H2DMG

Ni (HDMG)2 + 2H+
H

OH

CH3-C = N

N= C-CH3
+ 2H+

CH3 - C = N
2

+ Ni

2+

Ni

CH3 - C = N
CH3-C= N

N= C-CH3

OH
O

O
H

The precipitate is soluble in free mineral acids, in solutions containing more than 50
percent of ethanol by volume, in hot water (0.6mg per 100ml) and in concentrated
ammonical solutions of cobalt salts, but is insoluble in dilute ammonia solution., in
solutions of ammonium salts and in dilute acetic( ethanoic ) acid-sodium acetate
solutions.
Procedure: Weigh out accurately 0.3 to 0.4 g of nickel salt into a 500 ml beaker with a
stirring rod. Dissolve it in water, add 5 ml of dilute HCl (1:1) and dilute to 200 ml. Heat
to 70-80C, add a slight excess of dimethylglyoxime reagent, and immediately add dilute
ammonia solution dropwise, with constant stirring until precipitation takes place, and
then in slight excess .Allow to stand on the steam bath for 20-30 minutes, and test the
solution for complete precipitation when the red ppt has settled out. Allow the precipitate
to stand for 1 hour, cooling at the same time .Filter the cold solution through a sintered
-glass or porcelain filtering crucible, previously heated to 110 -120C and weighed after
cooling in a desiccator. Wash the precipitate with cold water until free from chloride (by
testing with AgNO3 to the filtrate) and dry it at 110-120C for 45-50 minutes. Allow to
cool in a desiccator and weigh. Repeat the drying until constant weight is attained as
Ni (C4H7O2 N2)2.
Yield:
Teacher's Signature:

Pharmaceutical analysis,Volumetry/Argenometry

:
Date: EXPERIMENT: TO DETERMINE THE PERSENTAGE PURITY OF
POTASSIUM BROMIDE

THEORY:
This experiment is the precipitation titration involving the precipitation reaction between
silver nitrate and sodium chloride.
AgNO3 + NaCl
2AgNO3 + K2 CrO4

Ag Cl + NaNO3
Ag2CrO4 + 2KNO3

A slight excess of AgNO3 solution reacts with indicator K2CrO4 and forms a reddish
brown color of AgCrO4. When Potassium Bromide is titrated against AgNO3 solution the
Br - ion is precipitated as silver bromide.
KBr + AgNO3

AgBr + K+ + NO3-

Firstly primary adsorbed layer is formed and it will hold the secondary adsorbed
oppositely charged ion presenting the solution .As soon as the equivalence point is
reached,Ag+ ions are present in the excess which are primarily adsorbed and nitrate ions
are secondarily adsorbed . During titration the eosin is used as indicator due to presence
of which the color of ppt. will change to the bright pinkish color at the equivalence point.
The -ve ions of eosin which are much more strongly adsorbed, than the nitrate ions are
immediately adsorbed and will reveal its presence of ppt. by formation of pinkish
complex of silver and a modified eosin ions, are on the surface with the first trace of Ag +
ions.

PROCEDURE:
1. Preparation of 0.05 M NaCl solution:
0.7455 gm of sodium chloride was taken by" weight by difference" method. It
was then transferred quantitatively to a 250 ml volumetric flask and was dissolved
in deionosed water, shaking continuously while adding to make the solution
homogeneous.
Molarity of the solution
2. Preparation of approx 0.05 M Silver nitrate solution:
2.122 gm of given Silver nitrate solution was made 250ml by adding deionosed
water.
3.

Standardization of the Silver nitrate solution with Sodium Chloride:

10 ml of Sodium Chloride solution was pipetted out in a conical flask. 1ml of 5 %
Potassium Chromate solution was added .Then it was titrated by slowly adding
silver nitrate solution from burette. The addition was continued with shaking till
the color becomes faint reddish brown. The titration was carried out and three
concurrent readings were noted.

4.

Determination of percentage purity of KBr:

0.835gm of potassium bromide solution was taken in 100ml of volumetric flask
and it was diluted by using deionosed water.
10ml of KBr solution was pipetted out in conical flask. Then 38 ml of deionosed
water, 1.5ml of 6M CH3COOH and 1ml of eosin (indicator) was added into
conical flask. It was then titrated with standard silver nitrate solution from burette.
The addition was continued with shaking till the color of ppt was pink.

OBESERVATION:
Table1: Standardization of Silver nitrate solution:
No. of obs.

Vol.of NaCl
(ml)

Burette readings for AgNO3(ml)

Initial

Final

Concurrent reading
(ml)

Difference

Table 2: Determination of weight of KBr in the given solution:

No. of obs.

Vol.of KBr
(ml)

Burette readings for AgNO3(ml)

Initial

Result:
Calculation:

Final

Difference

Concurrent reading
(ml)