University of Santo Tomas

Faculty of Pharmacy
PHA 6116 – Pharmaceutical Analysis I

PRACTICE SET: REDOX TITRATIONS

1. A solution of Na2S2O3 was standardized by dissolving 0.1210-g of KIO3 in water, adding a large excess
of KI and acidifying with HCl. The liberated I2 required 41.64-mL of the thiosulfate solution to decolorize
the blue iodostarch complex. Calculate the molarity of the Na2S2O3 solution.
Molar Masses: KIO3 = 214.0 Na2S2O3 = 158.1
Reaction: IO3-1 + 5I-1 + 6H + 1 → 3I + 3H2O
I2 + 2Na2S2O3 → Na2S4O6 + 2NaI
ANS: 0.08147M Na2S2O3

2. Exactly 33.31-mL of a KMnO4 solution were required to titrate a 0.1278-g sample of primary standard
Na2C2O4. What is the molarity of the KMnO4 solution? Molar Masses: KMnO4 = 158.0 Na2C2O4 = 134.0
Reaction: 5Na2C2O4 + 2KMnO4 + 8H2SO4 → K2SO4 + 2MnSO4 + Na2SO4 + 10CO2↑ + 8H2O
ANS: 0.01145M KMnO4

3. Determine the percentage of iron in a sample of limonite from the following data.
Molar Mass: Fe = 55.85 FeO = 71.84
Weight of sample: 0.5000-g
Volume of KMnO4: 50.0-mL (1.00-mL KMnO4 ≈ 0.005317-g Fe)
Volume of FeSO4: 6.00-mL (1.00-mL FeSO4 ≈ 0.00920-g FeO)
ANS: 44.6% Fe

4. Calculate the percent purity of copper in an ore in terms of Cu2O from the given data:
Molar Mass: KBrO3 = 167.0 Cu2O = 143.1
Weight of copper ore: 1.20-g
Volume of Na2S2O3 used: 40.00-mL (1.00-mL Na2S2O3 ≈ 0.004175-g KBrO3)
ANSWER: 35.8% Cu2O

5. A 5.00-mL sample of brandy was diluted to 1.00-L in a volumetric flask. The ethanol in a 25.00-mL aliquot
of the diluted solution was distilled into 50.00-mL of 0.02000M K2Cr2O7 where oxidation to acetic acid
occurred with heating:

Reaction: 3C2H5OH + 2Cr2O7-2 + 16H+1 → 4Cr+3 + 3CH3COOH + 11H2O

After cooling, 20.00-mL of 0.1253M Fe+2 was introduced into the flask. The excess Fe+2 was then titrated
with 7.46-mL of the standard K2Cr2O7 to diphenylamine sulfonic acid endpoint. Calculate the weight by
volume percent of C2H5OH in the brandy. Molar Mass: K2Cr2O7 = 294.2 C2H5OH = 46.07
ANSWER: 40.4% C2H5OH

PRACTICE SET: GRAVIMETRIC METHODS

1. Treatment of a 0.4000-g sample of impure potassium chloride with an excess of AgNO3 resulted in the
formation of 0.7332 g of AgCl. Calculate the percentage of KCl in the sample.
Molar Mass: AgCl = 143.32 KCl = 74.55
ANSWER: 95.5% KCl
 University of Santo Tomas
Faculty of Pharmacy
PHA 6116 – Pharmaceutical Analysis I

2. A 0.3516-g sample of a commercial phosphate detergent was ignited at a red heat to destroy the organic
matter. The residue was then taken up in hot HCl, which converted the P to H3PO4. The phosphate was
precipitated as MgNH4PO4·6H2O by addition of Mg2+ followed by aqueous NH3. After being filtered and
washed, the precipitate was converted to Mg2P2O7 by ignition at 10000C. This residue weighed 0.2161g.
Calculate the percent P in the sample. Molar Mass: Mg2P2O7 = 222.57 P = 30.974
ANSWER: 17.11% P

3. The mercury in a 0.7152-g sample was precipitated with an excess of paraperiodic acid, H5IO6, according
to the following reactions:
Reaction: 5 Hg+2 + 2 H5IO6 → Hg5(IO6)2(s) + 10 H+

The precipitate was filtered, washed free of precipitating agent, dried and found to weigh 0.3408-g.
Calculate the percentage of Hg2Cl2 in the sample. Molar Mass: Hg5(IO6)2 = 1448.75 Hg2Cl2 = 472.09
ANSWER: 38.82% Hg2Cl2