TABLE OF CONTENT

Abstract/Summary Introduction Aims/Objectives Theory Experimental Procedure Results Calculations Discussion Conclusion Recommendation References Appendices

PROCEDURES Experiment 1: Preparation of Calibration Curve for Conversion vs. Conductivity The reaction studied was the saponification reaction of ethyl acetate Et(Ac) and sodium hydroxide NaOH. Since this is a second order reaction, the rate of reaction depends on both concentrations of Et(Ac) and NaOH. However for analysis purposes the reaction was carried out using equimolar feeds of Et(Ac) and NaOH solutions with the same initial concentrations. Thus, both concentrations were ensured to be similar throughout the reaction. NaOH + Et(Ac) Na(Ac) + EtOH

PROCEDURES: 1. The following solutions were prepared: a. 1L of sodium hydroxide, NaOH (0.1M) b. 1L of ethyl acetate, Et(Ac) (0.1M) c. 1L of deionized water, H2O 2. The conductivity and NaOH concentration for each conversion values were determined by mixing the following solutions into 100mL of deionized water; a. b. c. d. e. 0% conversion 25% conversion 50% conversion 75% conversion 100% conversion : : : : : 100mL NaOH 75mL NaOH + 25mL Et(Ac) 50mL NaOH + 50mL Et(Ac) 25mL NaOH + 75mL Et(Ac) 100mL Et(Ac)

ANALYSIS AND DISCUSSION: 1. All data were recorded in the sample table in Appendix A. 2. The calibration curve of conversion vs. conductivity was plotted. The slope and y-axis intercept were determined.

Experiment 2: Back Titration Procedures for Manual Conversion Determination The manual conversion determination is carried out on experiment samples to verify the conductivity measurement values. The procedure explains the method used to carry out back titration on the samples. It was based on the principle of quenching the sample with excess acid to stop further reactions the back titrating with a base to determine the amount of unreacted acid. PROCEDURES: 1. The burette was filled with 0.1M NaOH solution. 2. 10mL of 0.25M HCl was measured in a flask. 3. 50mL sample was obtained from the experiment and immediately added to the HCl in the flask to quench the saponification reaction. 4. A few drops of pH indicator were added to the mixture. 5. The mixture was titrated with NaOH solution from the burette until the mixture was neutralized. The amount of NaOH titrated were recorded.

ANALYSIS AND DISCUSSION NaOH + HCl Unknown quantity; Concentration of NaOH in the reactor Known quantities; Volume of sample Concentration of NaOH in the feed vessel Volume of HCl for quenching Concentration of HCl in standard solution Volume of titrated NaOH Concentration of NaOH used for titration Calculations; Conc of NaOH entering the reactor, CNaOH,0 Volume of unreacted quenching HCl, V2 = = 1/2 CNaOH,f CNaOH,s * V1 CHCl,s mol/L mL = = = = = = Vs CNaOH,f VHCl,s CHCl,s V1 CNaOH,s mL mol/L mL mol/L mL mol/L = CNaOH mol/L NaCl + H2O

= Vol of HCl reacted with NaOH in sample, V3 = VHCl,s - V2 (CHCl,s * V3) / 1000 mL mol

Moles of HCl reacted with NaOH in sample, n1 Moles of unreacted NaOH in sample, n2 Conc of unreacted NaOH in the reactor, CNaOH

= =

n1 n2 / Vs * 1000

mol mol/L

= Conversion of NaOH in the reactor, X ( )

Experiment 3: Effect of Residence Time of the Reaction in a CSTR OBJECTIVE: To carry out a saponification reaction between NaOH and Et(Ac) in a CSTR To determine the effect of residence time onto the reaction extent of conversion To determine the reaction rate constant

PROCEDURES: 1. The general start-up procedures were performed. 2. Both pumps P1 and P2 were simultaneously switched on and valves V5 and V10 were open until the highest possible flow rate into the reactor was obtained. 3. The reactor was filled with both solutions until it was just about to overflow. 4. Valves V5 and V10 were readjusted until a flow rate of about 0.1L/min were obtained and that both flow rates were the same. The flow rate was recorded. 5. Stirrer M1 was switched on and the speed was set to about 200rpm. 6. The conductivity value at Q1-40 was monitored until it did not change over time to ensure that the reactor has reached steady state. 7. The steady state conductivity value was recorded and the concentration of NaOH in the reactor and the extent of conversion was calculated from the calibration curve. 8. Sampling valve V12 was opened and a 50mL sample was collected. Back titration procedure was carried out yo manually determine the concentration of NaOH in the reactor and extent of conversion. 9. The experiment from step 5 to 9 were repeated for different residence time by adjusting the feed flow ratesof NaOH and Et(Ac) to about 0.15, 0.20, 0.25, and 0.30L/min. Both flow rates were ensured to be the same. ANALYSIS AND DISCUSSION: 1. Graph of conversion vs. residence time was plotted. The reactors is defined as the reactor volume divided by the total feed flow rates. Residence time, 2. For a second order equimolar reaction with the same initial reactants concentration ( the rate law is shown to be:

Where: X CA F0 CA0

= extent of conversion = exit concentration of reactant NaOH (M) = total inlet flow rate of solutions (mL/min) = inlet concentration of reactant NaOH in the reactor (M)

3. Calculate the value of reaction rate constant, k and the rate of reaction for different reactor residence times.

RESULTS Experiment 1: Preparation of Calibration Curve for Conversion vs. Conductivity

Conversion (%) 0 25 50 75 100

V (Naoh) (Ml) 100 75 50 25 100

Conductivity (s/Cm) 9670 2580 1031 545 34

Naoh Concentration 0.05 0.0375 0.025 0.0125 0

Conversion vs. Conductivity

120 100 100

Conversion (%)

80

75

60 50 40 25

20

0 9670

2580

1031 Conductivity (s/cm)

545

34

Experiment 2: Back Titration Procedure for Manual Conversion Determination Reference Sample VNaOH (mL) Sample 1 25.3 0.1 2 27.9 0.15 3 28 0.2 4 24.5 0.25 5 24.4 0.3

Concentration of NaOH = 0.1M Concentration of HCL = 0.25

Experiment 3: Effect of Residence Time of the Reaction in CSTR Conductivity Flow Rate (L/min) 1 0.1 0.15 0.2 0.25 0.3 4.54 4.23 4.25 4.31 4.36 2 4.5 4.26 4.26 4.33 4.38 3 AVG 4.47 4.27 4.27 4.35 4.39 4.5 4.25 4.26 4.33 4.38 VNaOH (L) 32 29 27.5 25.5 24

320 193.3333 137.5 102 80

conversion vs.
120 100 80 60 40 20 0 320 193.3333333 137.5 102 80

conversion (%)