Experiment No.

Iodimetry

Assay of Antimony Potassium Tartrate, USP

I. Principle Involved
The assay of Antimony Potassium Tartrate employs a direct iodimetric titration using
0.1N Iodine VS. An oxidation reduction reaction takes place between the analyte and the
titrant resulting in the reduction of iodine to iodide and oxidation of the trivalent Antimony
to pentavalent Antimony. The indicator used is starch TS in which the appearance of a
persistent blue color indicates the endpoint of the titration. The titration must be carried
out in a mildly alkaline (pH 8) medium rendered by the addition of sodium borate.
II. Procedure
Dissolve about 500mg of Antimony Potassium Tartrate, accurately weighed, in 50mL of
water, add 5g of potassium sodium tartrate, 2g of sodium borate, and 3mL of starch TS, and
immediately titrate with 0.1N iodine VS to the production of a persistent blue color. Each mL
of 0.1N iodine is equivalent to 16.70mg of C 8H4K2O12Sb2·3H2O.
III. Official Requirement
Antimony Potassium Tartrate contains not less than 99.0 percent and not more than
103.0 percent of C8H4K2O12Sb2·3H2O.
IV. Clean-up Procedure
1. The titrated solution may be disposed into the sink.
V. Reasons for Important Steps
1. The sample must be dried to remove its water of hydration.
2. Potassium sodium tartrate is added to prevent the precipitation of basic salts of
antimony by hydrolysis. (). Precipitated salt of antimony would no longer be able to
participate in the titration, thus the results of the assay will be compromised.
3. Sodium Borate is added as a buffer to maintain the solution’s alkalinity. The mildly
alkaline condition for this assay is important because of several reasons:
a. The indicator used in this assay, starch, tends to hydrolyze or decompose in acidic
medium, thus, the end point may be affected.
b. The pH of the solution affects the reduction potential of the trivalent antimony.
KOOCCHOHCHOCHOHCOO(SbO) + I2 + H2O  KOOCCHOHCHOHCOO(SbO2) + 2H+ + 2I+
As seen on the equation above, when the H+ concentration is high, the equilibrium
is shifted to the left. Thus, employing an alkaline solution will prevent the left shift of
the reaction by neutralizing the hydrogen ions.
c. The iodide ions produced in the reaction tends to be oxidized by dissolved oxygen in
the acid solution.
4I- + O2 + H+  2I2 +H2O
Since in an alkaline medium, the hydrogen ions are neutralized, there will be no
hydrogen ions to participate in the reaction above.
 d. The solution must only be mildly alkaline (pH 8) and not too alkaline because iodine
will disproportionate to hypoiodate and iodide.
4. 0.1N Iodine VS is the titrant due to its moderately strong oxidizing property.
5. Starch is the indicator used in this assay because when all the trivalent antimony have
been oxidized to pentavalent antimony, iodine will consequently not be reduced to
iodide and starch will be able adsorb iodine, forming a persistently blue colored
solution.
B13 +