Date: Experiment No 9 Determination of K A by Sulphite Oxidation Method
Date: Experiment No 9 Determination of K A by Sulphite Oxidation Method
Date: Experiment No 9 Determination of K A by Sulphite Oxidation Method
Experiment No 9
AIM:
To determine the oxygen mass transfer coefficient, KLa using sodium sulphite oxidation
method.
THEORY:
The volumetric liquid mass transfer coefficient (KLa) is a useful parameter to characterize
bioreactors capacity for aeration. This helps the reactor design, optimization of technologies and
scaling up or scaling down processes. The sodium sulphite combines with oxygen to give sodium
sulphate, with CuSO4 as catalyst in the reactor. The concentration of sodium sulphite at various
time points is inversely proportional to the oxygen transfer rate.
Cu2+
Na2SO3 + ½ O2 Na2SO4
The above reaction is
A. Independent of sodium sulphite concentration within the range of 0.04N to 1.0N
B. The rate of the reaction is much faster than O2 transfer rate.
Thus, the rate of oxidation is controlled by rate of mass transfer alone.
The reaction consumes oxygen at a rate that is sufficiently fast so that transport of O2 from gas to
liquid through liquid film is the rate-limiting step. The rate of the reaction is zeroth order in
Na2SO3. If the reaction is not fast enough the reaction occurs in the liquid film around the gas
bubbles. This would decrease apparent film thickness and give incorrectly high values of K La.
Concentrations of unreacted sulphite are determined by reacting the sulphite with excess iodine
and then back titration of the iodine with thiosulphate. It is important to note that the dissolved
oxygen is zero through the reaction.
By titrating sodium sulphite present in the reactor (by taking sample at fixed intervals of time)
against sodium thiosulphate, the quantity of sodium sulphite that would have reacted according
to equation can be measured as the difference between successive rate instants of time. Then
based on stoichiometry the corresponding number of moles of O2 that would have been
consumed can be determined.
The Oxygen transfer rate
OTR = KLa (C*-CL)
Where C* = 8.43X10-3g/l at 25oC
CL = Dissolved Oxygen content.
In this case, CL = 0, since the DO is maintained such that it is not saturated.
OTR = KLa (C*) -------- (1)
KLa = OTR/ C*
Thus KLa can be determined.
MATERIALS REQUIRED:
0.5M Na2SO3
1% starch solution
0.5M Na2S2O7
0.002M CuSO4.5H2O
Standard Na2SO3 (0.1M to 0.5M)
0.1M Iodine solution (20 g/l KI + 12.7 g/l I2)
Measuring cylinder
Distilled water
Test tubes, eppendorfs, Burette, Conical flask, Magnetic stirrer etc.
PROCEDURE:
100 ml of 0.5M Sodium sulphite & 0.002M Copper sulphate solutions were taken in a
250ml conical flask.
The conical flask with Sodium sulphite solution was kept in magnetic stirrer for mixing
and ‘0’ sample was taken for titration.
15 mL of Iodine solution and few drops of starch indicator was added to the 1 ml of
sample was taken from the flask.
Sample solution was turned into dark blue colour and it was titrated against 0.5 N Sodium
thiosulphate. (It becomes straw yellow color)
The volume consumed are been noted.
The same analysis has been repeated for the time of 5, 10, 15, 20 minutes samples.
Graph was plotted between titer volumes versus time.
OTR was calculated by using the slope of the graph.
KLa value was calculated by using OTR & C* values.
TABLE 1:TITRATION
MODEL GRAPH:
CALCULATION:
RESULT: