Lab Exp 3

Name: Trần Quang Hưng
Class: K65 Advanced Chemistry
Redox Oxidation
Part 1: Redox oxidation with Potassium Permanganate and Dichromate
Determination of Iron in Ore
A. Redox Titration with Potassium Permanganate.
* Experimental procedure
1. Standardization of potassium permanganate solution:
The standardization and the determination of the unknown should each be based on at
least three titrations. After your first determination, it is preferable to use the procedure
described in
Procedure: Weigh about 0.2 g Na2C2O4 (to the nearest 0.1 mg) (for this experiment we
weigh about 0.298g Na2C2O4) and put a sample into a 400 mL beaker. Dissolve each
sample in about 250 mL of 1 M H 2SO4. Heat each solution to 80 - 90 °C, and titrate
with KMnO4 while stirring with a thermometer. The pink color imparted by one
addition should be permitted to disappear before further titrant is added. The
temperature should not drop below 60 °C. The end point is marked by the appearance
of a faint pink color that persists at least 30 s. Determine a blank by titrating an equal
volume of the 1 M H2SO4. Correct the titration data for the blank, and calculate the
concentration of the permanganate solution.
=> V = 18mL
2. The determination of iron in an ore:
Add 10 mL of Zimmerman - Reinhard reagent (Caution! This is a caustic mixture
containing concentrated sulfuric acid and phosphoric acid.) and 100 mL of water.
Titrate immediately with standard KMnO4 to the first faint pink that persists for 15
to 20s. Do not add the KMnO 4 rapidly at any time. Correct the titrant volume for
the blank if it has been determined.
First titration: V = 10.5 (mL)
Second titration: V = 10.7 (mL)
=> average Volume is 10.6 (mL)
B. Determination of iron using potassium dichromate: Redox indicators
*Experimental procedure
Titration with K2Cr2O7
Add 8 drops of diphenylamine sulfonate indicator and slowly titrate with your standard
K2Cr2O7 solution from a blue-green, through a greyish tinge to the first permanent
violet, which is the end point. The titration should be conducted dropwise when the
grey tinge is noted because the oxidation of the indicator is somewhat slow at this
point. Do a trial run first to see the end point and determine the sample weight. Then
do three good trials. The average standard deviation should not exceed 0.02 mL.
=> m(K2Cr2O7 )= 0.29 (g)
First run: V(K2Cr2O7 )=7.4(mL)
Second run: V(K2Cr2O7 )= 7.41 (mL)
Part 2: Iodometric determination of copper in brass

III. Experimental Procedure:
1. Standardization of Na2S2O3 solution:
Pipette accurately Vml (10.00ml) of K 2Cr2O7 solution of known concentration into

a 250ml conical flask. Add 5ml of 3M H2SO4, 10ml of 5% KI solution, shake
gently, cover the mouth of the flask with a watch glass and let stand in the dark
for 10 minutes. Then titrate the amount of I2 released with Na 2S2O3 solution until
the solution is straw yellow, add 1ml of 1% starch paste, shake well and titrate
further until the blue color disappears. Record the number of ml of titrated
Na2S2O3 solution - V0ml. Do it 3 times and average the results.
First titration: V1(Na2S2O3)= 8(mL)

Second titration: V2( Na2S2O3)= 12.2 (mL)
2. Titration of Cu-Brass Solutions
Take 10.0 ml of solution A into a 250 ml conical flask. Add 10 ml of 5% KI
solution (in KSCN), shake gently, cover the mouth of the flask with a watch glass
and let stand in the dark for 10 minutes. Titrate the I2 produced with Na2S2O3 C1
solution (mol/l) of known concentration until the solution is straw yellow, then add
1ml of 1% starch solution (the solution turns blue-violet). Continue titration until
the solution loses its blue color. Titrate until the starch-blue color begins to fade.
Add 1 g of potassium thiocyanate, KSCN, and complete the titration. (I 2 tends to
adsorb strongly on the solid CuI precipitate. Thiocyanate is added to displace the
adsorbed I2 making it accessible to the starch colloidal particles, hence yielding a
sharper endpoint.). Record the number of ml of Na2S2O3 titrated - out of V1 ml.
=> V Na2S2O3 = 34.7mL

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Lab Exp 3

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Name: Trần Quang Hưng

Class: K65 Advanced Chemistry

Titration with K2Cr2O7

Part 2: Iodometric determination of copper in brass

Pipette accurately Vml (10.00ml) of K 2Cr2O7 solution of known concentration into

First titration: V1(Na2S2O3)= 8(mL)

=> V Na2S2O3 = 34.7mL

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