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ABSTRACT There are three objectives that must be achieved in order to complete this experiment.

First, to studied the saponification reaction of ethyl acetate Et(Ac) and sodium hydroxide NaOH. Secondly, to study the effect of residence time onto the reaction extent of conversion and for the last objective that is to determine the reaction rate constant. To determine the theoretical value of the reaction extent of conversion, the calibration curve experiment must be done first to be compared with the experimental value obtained. For the next experiment, the residence time and the conversion percentage need to be calculated in order to obtain the rate constant. After all that calculation done, then the graph of conversion versus residence rate can be plotted. Unfortunately, the graph of conversion versus residence time is not successfully done referring to the theoretical as there are a few errors occur during the experiment. Even though this experiment is successfully complete but the objectives are not done completely.

INTRODUCTION Ideal stirrer-tank reactor. Continuous Stirrer-Tank Reactor (CSTR) usually runs at steady state with continuous flow of reactants and products, the inlet and outlet has the same amount of composition as in the reactor. The rate of the inlet and outlet streams inside of the reactor must be more accessible than any other reactors. There is an inlet stream(s) that bring all of the reactants in at a particular rate. This stream(s) dumps into a large container; there is a shaft with a blade attached (stirrer) in the reactor that rotates around to mix the reactants. Finally there is an outlet stream, which the solution will exit from the reactor. Also because of the simplicity of the components involved in the reactor, the maintenance is easy and cheap. It also does not require much work to keep running. It takes more space to mix the components in comparison to other reactors. In industrial sector, it is used when relatively small amount of material are to be treated. In reactor design we have to know what size and type of reactor and method of operation that best for a given job. This may require the conditions in the reactor vary with position as well as time; this question can only be answered by a proper integration of the rate equation for the operation. This may pose difficulties because the temperature and composition of the reacting fluid may vary from point to point within the reactor, depending on the endothermic or exothermic character of the reaction, the rate of heat addition or removal from the system, and the flow pattern of fluid through the vessel. Briefly indicate the particular features and the main areas of application of these reactor types. There are many other types of reactors out there. For example, in a batch reactor there is reactants put in a container and the container is closed for a period until the reaction is done. It is used for small-scale operation, for testing new process that have not been fully developed, for manufacture of expensive products, and for processes that are difficult to convert to continuous operations. Besides that, it has the advantage of high conversions that can be obtained by leaving the reactant for long periods of time. It also has the disadvantage which is it has a high costs per batch and the difficulty of large-scale production.

AIMS 1. To studied the saponification reaction of ethyl acetate Et(Ac) and sodium hydroxide NaOH 2. To study the effect of residence time onto the reaction extent of conversion 3. To determine the reaction rate constant THEORY

PROCEDURE General Start-Up Procedures 1. The following solutions were prepared 40 L of sodium hydroxide, NaOH (0.1M) 40 L ethyl acetate , Et(Ac) (0.1M) 1 L of hydrochloric acid, HCL (0.25M), for quenching

2. All valve were initially closed 3. The vessel were change as followed The charge port cap of vessels B1 and B2 were opened NaOH and Et(Ac) solutions were pour into vessels B1 and B2 accordingly The charge port cap for both vessels were closed

4. The power was turn on 5. The water in the thermostat T1 tank was check from time to time to see if there are sufficient water during the experiment 6. The overflow was adjusted to give a working volume of 10L in the reactor R1 7. Valves V2,V3,V7,V8 and V11 were opened General Shut-Down Procedures 1. Pump P1 and P2 and stirrer M1 were switch off 2. Thermostat T1 was switch off and the liquid in reaction vessel R1 was cool down to room temperature 3. Valves V2, V3, V7, V8 and V11 were closed. Valves V4, V9 and V12 were opened to drain any liquid from the unit 4. The control panel was turn off

Experiment 1: Preparation of Calibration Curve for Conversion vs Conductivity 1. The following solution were prepared: 1 L of sodium hydroxide, NaOH(0.1M) 1 L of sodium acetate, Et(Ac) (0.1M) 1 L of deionised water, H2O

2. The conductivity and the concentration of NaOH for each conversion values by mixing the following solutions into 100 mL of deionised water were determined: 0% conversion 25% conversion 50% conversion 75% conversion 100% conversion : 100 mL NaOH : 75 mL NaOH + 25 mL Et(Ac) : 50 mL NaOH + 50 mL Et(Ac) : 25 mL NaOH + 75 mL Et(Ac) : 100 mL Et(Ac)

Experiment 2: Effect of Residence Time of the Reaction in a CSTR 1. General start-up procedures were formed 2. Pump P1 and P2 were switch on simultaneously and valve V5 and V10 were opened to obtain the highest possible flow rate in the reactor 3. The reactor was fill with both solutions until it just about to reach overflow 4. Valve V5 and V10 were readjusted to give a flow rate of 0.1 L/min. 5. Stirrer M1 was switch on and the speed was set at 200 rpm 6. Conductivity value was monitored at QI-401 until it does not change. This is to ensure that the reactor is in steady state 7. The conductivity value was recorded and the concentration of NaOH and extent of conversion from the calibration curve were determined 8. Valve V12 was opened and 50 mL of sample was taken. Back titration was carried out manually in order to determine the concentration of NaOH in the reactor and extent of conversion 9. Experiment was repeated (step 5 to 9) for different resident times by adjusting the feed flow rates of NaOH and Et(Ac) to about 0.15, 0.20, 0.25 and 0.30 L/min.

RESULT AND CALCULATION Experiment 1

Conversion (%) 0 25 50 75 100

Solution mixture (mL) 0.1M NaOH 100 75 50 25 0 0.1M Et(Ac) 0 25 50 75 100 H2O 100 100 100 100 100

Concentration of NaOH (M) 0.0500 0.0375 0.0250 0.0125 0

Conductivity (ms/cm) 7.02 4.88 2.46 1.15 0.147

120

CONDUCTIVITY VERSUS CONVERSION

100

80 Conversion (%)

60 y = -13.887x + 93.484 R = 0.9707

40

20

0 0 -20 1 2 3 4 Conductivity (ms/cm) 5 6 7 8

Experiment 2 Reactor volume Concentration of NaOH in feed vessel Concentration of Et(Ac) in feed vessel = 10 L = 0.1 M = 0.1 M

Bil

Flow rate of NaOH(L/mi n)

Flow rate of Et(Ac),(L/ min)

Total flowrate of solutions, V0,(L/min)

Residence time, (min)

Conductivity (ms/cm)

Conve Exit concentra rsion, X (%) tion of NaOh, CNaOH (M) 2.8x10-3 2x10-3 -1x10-3 9.2x10-3 3x10-3 94.4 96 102 81.6

Rate constant,k (mol/L.mi n)

1 2 3 4

0.10 0.15 0.20 0.25

0.10 0.15 0.20 0.25

0.20 0.30 0.40 0.50

50.0000 33.3333 25.0000 20.0000

2.87 2.67 2.62 2.61

120.4082 240 1020 9.6408

0.30

0.30

0.60

16.6667

2.65

94

104.44

Bil 1 2 3 4 5

Flowrate(mL/min) 0.10 0.15 0.20 0.25 0.30

Volume of titrated NaOh(mL) 23.6 24.0 25.5 20.4 23.5

120 100 Conversion,X (%) 80 60 40 20 0 0 1

Conversion versus residence time

y = -1.52x + 98.16 R = 0.1045

3 Residence time, (min)

SAMPLE CALCULATION Volume of sample Conc. Of NaOH in feed vessel, CNaOHf Volume of HCl for quenching, VHCls Conc. of HCl in standard solution, CHCls Volume of titrated NaOH, V1 Conc. Of NaOH used for titration, CNaOHs = 50 mL = 0.1 mol/L = 10 mL = 0.25 mol/L = 24.4 mL =0.1 mol/L

Concentration on NaOH entering the reactor,

At flow rate=0.10ml/min

Conversion of NaOH in reactor,X

Residence time,

Reaction rate constant,k

DISCUSSION This report consists of two experiments which contain some objectives that need to be considered. Which are to carry out the saponification reaction of ethyl acetate Et(Ac) and sodium hydroxide NaOH, to study the effect of residence time onto the reaction extent of conversion and for the last objective that is to determine the reaction rate constant. In the first experiment, the calibration curve is carried out by using the pure sample of NaOH, distilled water and ethyl acetate. Each sample is mixed together without the same concentration and volume to obtain the conductivity of the conversion, X. Calibration curve is a method to determine the concentration of a substance in an unknown sample by comparing it to a set of standard samples of known concentration. In addition, the conversion of compound or mixture in the reactor can be determined. From the graph, it shows that as the conductivity decreased, conversion increased. The value for the slope is -13.887 while for the y-intercept is 93.484.Thus, as the conversion increased, the conductivity decreased. For the second experiment, the feed flow rate of each solution can be adjusted at the instrument, to get the sample of solution before being titrated. Then, the volume of NaOH titrated with the sample solution is jot down. Later, the residence time value for each total feed flow rates can be calculated. For the first flow rate, the residence time is 1.68571 while for the conversion is, 94.4%. Unfortunately while conducting this experiment, several errors occur that disrupt the reading of the NaOH titrated. The experimental and calculation value of the conversion should vary with the theoretical value based on the calibration curve as shown below,
57 56.5 56 conversion,(%) 55.5 55 54.5 54 53.5 2.55 2.6 2.65 2.7 2.75 Conductivity (ms/cm) y = -8.8576x + 79.334 R = 0.9224 2.8 2.85 2.9

Conversion versus conductivity

As the conductivity increased, the conversion value increased too. However, at flow rate 0.30ml/min, the conductivity is decreasing which opposing the calibration curve slope value. This might occur during adjusting the flow rate that influences the conductivity value. The residence time value for each flow rate is obtained by calculation, volume of the reactor divide with the feed flow rate. Overall, the value for the residence times are consistent as the volume of the reactor is fixed as well as the difference between each flow rate also consistent, 0.10l/min. Even though the residence time values are correct, but the conversion value is not accurate as there are errors occur at the volume of NaOh titrated. This might occur during the titration of the sample using phenolphthalein and NaOh. The valve of burette is not control carefully that making the color of not as light as light pink in the mixture during titration. Furthermore, the color of the titrated sample is not the same, light pink along the titration process for each of the flow rate. In this experiment, there are some precautions that should be taken during the experiment to reduce the erroneous and get more accurate results in the experiment. There are some aspects in this experiment that can be improved. First, control the valve of burette to make sure that the color of light pink in the mixture is the same during titration. Second, avoid the parallax reading to avoid the error by putting the paper to the same level of solution at the back of burette for easier reading. Third, make sure all the apparatus are washed cleanly before being used to reduce the erroneous in this experiment.

CONCLUSION As conclusion, both experiments are not done successfully as errors occur during the experiment. For the experiment 1, it can be seen that the calibration graph plotted is quite same as shown in the theory part. But for experiment 2, the graph plotted was different from the theory as the slope is different from the theory. This is because of a few errors occurring during the experiment. Lastly, the objectives of this experiment are not achieved completely. RECOMMENDATION 1. Make sure the flow rate of both vessels that enter the reactor is the same 2. Make sure that the mixing is in steady state before taking out the sample 3. make sure no bubbles trapped in the piping because it will affect the readings of the conductivity(for first experiment) 4. To avoid overflow, do not use too high flow rate 5. Rinse all the apparatus carefully before it was used because it can interrupt the results

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