DISCUSSION

The aim of this experiment is to investigate about saponification reaction by using Continuous
Stirred Tank Reactors (CSTR) 40L. This experiment has been conducted to carry out
saponification reaction between NaOH and Et(Ac) to determine the effect of residence time
onto the reaction extent of conversion and the reaction rate constant. CSTR is a type of reactor
where the contents are uniform throughout the reactor due to its well-stirred nature. The reactor
variables can be estimated as the CSTR model itself is used to predict the behaviour of chemical
reactors. Meanwhile the saponification process itself, is a process to make soap and it is one of
the continuous reaction. It is a process by which triglycerides are reacted with sodium or
potassium hydroxide (NaOH or KOH) to produce glycerol and fatty acid salt called soap, where
in this experiment, the reaction of saponification is quenching with hydrochloric acid to stop
the reaction. The reaction quickly reacts, and back titration is done to investigate the volume
reacted.
From the data collected and calculated from the experiment, three graphs need to be plotted
which are conductivity versus conversion for manually conversion experiment and conversion
X versus residence time for reaction in CSTR. In addition, calibration curve, (graph 1) also
need to be plotted as the conductivity of the reaction between NaOH and Et (Ac) at certain
percentage of conversion need to be determined. The y-intercept from the graph is determined
at 106.66% conversion. The reaction of saponification in this experiment is process that based
on the principle of quenching the sample with excess acid (hydrochloric acid) to stop further
reactions then back titration is used to determine the amount of unreacted acid. From the
calculation, it is proven that when the volumetric flow rate decreased, the value of conversion
is increased. All the calculated data had proved that the theory form from the calibration curve.
From graph 2, we can see that the conversion, X decrease proportionally as the total flow rate
increased. The conductivity meanwhile did not show pattern in the data collected as the value
of conductivity decreased from total volume flowrate of 100 to 200 mL/min and then start to
increase until 600 mL/min. The graph plotted is not as expected from the theory which the
conductivity should be decreased as the total volume flowrate increased. This is because when
fluid entering the reactor at time t, it will exit at time t + , as the residence time, is time that
the fluid elements spend within reactor. The higher the flow rate, the time of reactant spend
time in the reactor should be lesser than lower flow rate. The slight error in the experiment lead
to the result error. The experiment can be successfully done if some of the error can be avoided.
The total volume flow rate need to be accurate as we need to always keep our eye on the valve
V5 and V10 to get the constant and similar flow rates of both NaOH and Et (Ac). The valve, if
not controlled can lead to the non-accurate reading of the conductivity. From graph 3, which is
conversion versus residence time, we can conclude that the conversion increased as the
residence time increased. The highest conversion, 98.2% occur at the highest residence time
which is 45 min. From the calculated result, the reaction rate constant is decrease as the
volumetric flow rate is increase. And when the reaction rate constant increase, the rate of
reaction will decrease. The rate of reaction is highest which is rA= 0.00133 mol/L.min at the
lower rate constant which is k = 39.42 L/mol.min. the reaction is second order and the rate law
is rA = kCACB. The higher the k value, more volume of NaOH require to convert a mole of
NaOH in 1 second.
CONCLUSION
As a conclusion, the objectives of this experiment are to determine the effect of residence time
onto the reaction extent of conversion as well as reaction rate constant. The reaction rate
constant is well determined and recorded as a data in the result section. As we can see, the
highest reaction rate constant is 606.17 L/mol.min when the flowrate is 200 mL/min. The
lowest reaction rate constant, which is 39.42 L/mol.min occur when the flowrate is 600
mL/min. We can conclude that the higher the flowrate, the lower the reaction rate constant.
From the graph conversion versus residence time, we can conclude that the conversion
increased as the residence time increased. Lastly, the rate of reaction will decrease, if reaction
rate constant increased.

RECOMMENDATION
The percentage of the error will be minimized during this experiment as long as there are some
recommendations as to improve the performance and precaution being considered during the
experiment.

During this experiment, some errors were found out that affect the performance of the reaction
process. It is recommended that the sample is supposedly titrated immediately since the
conversion is calculated from the titrated sample. Due to late titration of the sample, the
samples start to decompose then affect the conversion value. Furthermore, titration should be
immediately stopped when the indicator turned light pink because it is the point where it
reached equivalent point. In addition, when the sample is being collected, the first millimetres
should be thrown away, for it is the remaining of the previous sample trapped in the pipe. The
total volume flow rate need to be accurate as we need to always keep our eye on the valve V5
and V10 to get the constant and similar flow rates of both NaOH and Et (Ac). The valve, if not
controlled can lead to the non-accurate reading of the conductivity. It is recommended that the
time taken for taking sample is increased so that the conversion value will be higher. Follow
the concept of CSTR, the longer the time the higher the conversion value. During conducting
experiment, the safety precaution especially wearing all PPE should be applied so that any
accident during experiment will be prevented.