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BACKGROUND
Several points require attention when using MnO4- as the titrant. Under certain
conditions, the MnO4 - can oxidize chloride to chlorine, requires special measure.
Permanganate solutions, especially dilute ones, are not very stable for storage. In addition,
the reduction of MnO4 - may proceed to different oxidation states of Mn, depending on the
solution condition.
1. Weigh 1.6 g of potassium permanganate to the nearest hundredth of a gram and dissolve
in 500 mL of deionized water in a 1L beaker.
2. Heat the solution to boiling, keep hot for about 30 minutes over low heat and then allow
it to cool. Heating of the solution hastens the oxidation of any organic matter present and
also aids in the coagulation of the Mn(IV) oxides.
3. Filter through a sintered glass or porcelain filter of the fine porosity under suction. Care
should be exercised to perform all operation with clean glassware and with precautions that
no additional organic matter such as particles from rubber stopper or tubing is introduced.
Under no circumstances, of course, use filter paper for filtration.
4. Transfer the filtrate to a clean, glass-stopper bottle and store in the dark.
Anhydrous sodium oxalate, Na2C2O4, is available in high purity and is stable in air.
For the standardization of permanganate solution, an accurately weighed amount of this salt
is dissolved in sulfuric acid and titrated with the permanganate solution. In the acidic
medium the oxidation is best described in terms oxalic acid:
H2C2O4 → 2 H+ + 2 CO2 + 2 e-
The overall reaction between permanganate ion and oxalic acid may be expressed as
2 MnO4- + 5 H2C2O4 + 16 H+ → 2 Mn2+ + 10 CO2 + 8 H2O
When permanganate is first added to a solution of oxalic acid, the solution immediately
becomes pink and remains so for some time, indicating the slowness of the reaction. As the
titration is continued, the decolorization becomes rapid, because the Mn2+ formed by the
reaction catalyzes the reduction of permanganate ions. In the vicinity of the end point the
decolorization is almost instantaneous.
2. Transfer the salt quantitatively to a 250 mL volumetric flask, add about 200 mL of DW,
swirl until complete dissolution, and dilute to mark and mix well.
1. Transfer 25.00 mL of sodium oxalate standard solution into an Erlenmeyer flask, and add
20 mL of 1:10 sulfuric acid and then 75 mL of water.
2. Heat the solution slowly on a hot plate, with stirring, to about 80 °C (use a thermometer
to determine temperature, but not as stirring rod!)
3. Remove the beaker from the hot plate and begin the titration with the 0.02 M potassium
permanganate. Add the initial portions of titrant slowly, allowing complete decolorization to
occur before the next portion is added. Note the temperature from time to time; if it falls
below 70 °C, reheat the solution. Titrate until a faint pink is attained that persists for at least
20 seconds.
4. Establish a blank by bringing 120 mL of water and 20 mL of 1:10 sulfuric acid to the
same persistent pink by the addition of the titrant solution.
5. Take the blank into account and calculate the molarity of the permanganate solution
6. Repeat the titration with at least two additional aliquots of the oxalate standard solution.
7. Calculate the average molarity and standard deviation (< 0.5% rsd) of at least three
results.
A permanganate titrant serves well for the determination of hydrogen peroxide even
in dilute solutions. As in the titration of oxalic acid, the decolorization of the initial portion
of titrant added may be somewhat slow. Since hydrogen peroxide decomposes at an
elevated temperature the titration should be performed at room temperature.
1. Receive your sample (5 mL) in a well-cleaned 50 mL beaker. Keep a watch glass over the
top of the beaker to prevent contamination. Because of the low stability of hydrogen
peroxide sample, the titration must be performed during the laboratory period in which the
sample is received; preferably all arrangements for the titration should be completed before
the sample is issued.
2. Pipet a 1.00 mL of aliquot of the sample solution into an Erlenmeyer flask, dilute with
100 mL of water, and add 20 mL of 1:3 sulfuric acid.
3. With gentle swirling of solution, titrate with permanganate solution until a faint pink is
attained that lasts for at least 30 seconds.
4. Establish a blank by titrating 100 mL of water and 20 mL of 1:3 sulfuric acid to the same
pink color.
5. Take the blank into account and express the titration result as grams of hydrogen
peroxide present in 100 mL of the sample.
6. Repeat the titration at least twice and calculate the average and percent relative standard
deviation of your result.
QUESTIONS
3. Write the equation for the decomposition of hydrogen peroxide and the equations for the
two half-reactions involved.