ABSTRACT

APPARATUS

1.

Armfield Chemical Reactor Service Unit

2. Armfield Continuous Stirred Tank Reactor (CSTR) 3. Feed Vessels (2) 4. Sample Beakers (2) 5. Temperature / Conductivity Probe 6. Overflow Container 7. Tubes and Connections 8. Temperature / Conductivity Convertor 9. Computer with CSTR software package 10. Syringe and tube 11. Electronic Balance Chemicals 12. Anhydrous NaOH pellets 13. Distilled Water

Figure 1: CSTR apparatus setup

PROCEDURE 1. The power switch of the chemical reactor service unit was turned. It was ensured that the three circuit breakers and the RCCB on the rear of the unit are in the UP position. The computer was turned on. 2. The CSTR icon on the Windows desktop was double-clicked. The basic features of the Armsoft package, especially the mimic diagram, graph and data table was observed carefully by the experimenter. 3. The reagent vessels were filled with distilled water when necessary and the feed pumps and the agitators were set for manual operation. 4. The speed of the feed pump #1 was gradually increased by rotating the speed dial clockwise until the NaOH Flow reading on the mimic diagram was approximately 82ml/min. The speed of the feed pump #2 was gradually until the EtAc flow reading was around 82ml/min. 5. The water from the CSTR was allowed to build up until it reached the top of the standpipe and the effluent started to flow to drain through the attached plastic tubing. The drain tubing was placed into a small beaker and the conductivity probe was inserted into

the beaker. The speed of the agitator was increased until the Stirrer Speed field on the mimic diagram showed an increase of 200rpm. 6. View data in graph format tab was selected and Run #1 Measured Conductivity (mS) on the primary y- axis was trended. The View diagram tab was returned to and the button configure was left clicked. The sampling intervals were fixed at 10seconds. OK was clicked to close the dialog box then Sample Start. 7. A 7.5 M sodium hydroxide solution was made up by dissolving 7.5 g of sodium hydroxide pellets into 25ml of distilled water. The solution was allowed to reach room temperature. 8. A 10ml syringe was filled the tracer solution. The piece of flexible tubing was lowered through the conductivity gland until it nearly touched the bottom of the reactor and the syringe was inserted. The solution was quickly injected and the flexible tubing was withdrawn. 9. The conductivity readings were observed (it was measured at the exit of the vessel) as it was plotted in real time on the computer. 10. When the initial conductivity that was measured returned to its initial value, the agitator was turned off and steps 8-9 was repeated. 11. When the experiment was completed, the data collection was stopped by clicking the Stop Sample button. The results were saved in Formula One and Excel formats. 12. The controls on the reactor service unit were set to minimum/off and the unit was turned off. The contents of the CSTR was drained into a 2 litre graduated cylinder and the volume of the liquid was measured. RESULTS Table 1: Measured and Calculated Results Agitator On (200 rpm) Volume (ml) Volumetric Flow Rate(ml/min) Mean Residence Time/s (based on V/v) Mean Residence Time/s (Based on RTD measurements) Number of Tanks, N Agitator Off (0 rpm)

726.59 1.64

1159.45 2.73

SAMPLE CALCULATIONS DISSCUSSION SOURCES OF ERROR PRECAUTIONS SAFETY CONSIDERATIONS