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Assay of Antimony Potassium Tartrate

This experiment involves the iodimetric titration of antimony potassium tartrate using 0.1N iodine solution. An oxidation-reduction reaction occurs between the analyte and titrant, oxidizing trivalent antimony to pentavalent antimony and reducing iodine to iodide. Starch indicator is used to detect the endpoint, which is a persistent blue color. The titration must be done under mildly alkaline conditions using sodium borate to buffer at pH 8 for accurate results.

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4K views2 pages

Assay of Antimony Potassium Tartrate

This experiment involves the iodimetric titration of antimony potassium tartrate using 0.1N iodine solution. An oxidation-reduction reaction occurs between the analyte and titrant, oxidizing trivalent antimony to pentavalent antimony and reducing iodine to iodide. Starch indicator is used to detect the endpoint, which is a persistent blue color. The titration must be done under mildly alkaline conditions using sodium borate to buffer at pH 8 for accurate results.

Uploaded by

Tricia So
Copyright
© Attribution Non-Commercial (BY-NC)
We take content rights seriously. If you suspect this is your content, claim it here.
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Experiment No. 8 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. 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 C8H4K2O12Sb23H2O. Official Requirement Antimony Potassium Tartrate contains not less than 99.0 percent and not more than 103.0 percent of C8H4K2O12Sb23H2O. Clean-up Procedure 1. The titrated solution may be disposed into the sink. 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 solutions 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+

II.

III.

IV. V.

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 +

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