CPE554

Universiti Teknologi MARA

A. General Start-Up Procedures 1. Ensure all valves are closed. 2. Turn on the power for the control panel. 3. Prepare a 3040 L mixture containing ethanol and filtered water at the desired composition. Charge the unit as follows: i. Open the charge port cap at the reboiler B1, and fill the reboiler up to the level of the internal overflow height. ii. Pour the remaining ethanol-water mixture into the feed vessel B2 through the feed charge port. 4. Set the reflux divider KFS-101 to total reflux. This is to prevent any distillate from escaping when starting up the distillation column. 5. Let the cooling water flow into the condenser W2 and product coolers W3 & W4 by opening valves V13, V14 and V15. 6. Ensure that the tip of the level switch is located below the reboiler equator, which is at the liquid inlet from the cartridge heaters. 7. Switch on the cartridge heaters at W1. Allow the liquid in the reboiler to boil. 8. Observe the vapor rising from the boiling liquid into the distillation column. As the vapor reaches the condenser, it will condense and flow back into the column as liquid. Mass transfer will take place between this liquid and vapor phase in the column. 9. Check that the condenser has sufficient cooling water flow to minimize escape of vapor into the vent. 10. Let the distillation column run until a stable condition is observed. The stable condition is reached when all temperature indicators on the column give a constant reading with an allowable fluctuation of 0.2C.

B. General Shut-Down Procedures 1. Set the reflux divider KFS-101 to total reflux. 2. Keep the cooling water running through the condenser W2 and product coolers W3 & W4. 3. Switch off the cartridge heaters W1. Monitor the temperature drop in the reboiler. Wait until it has cooled down to less than 50C. 4. Close the cooling water valves V13, V14 and V15. 5. Drain all liquid from the reboiler B1 and product vessels B3 and B4 by opening valves V6, V9 and V12. Also drain the liquid in the pipelines by opening valves V5, V8, V10 and V11. The liquid can be re-mixed and recycled for future use. 6. Turn off the power for the control panel.

Exp/Distillation Column

CPE554

Universiti Teknologi MARA

C. Sampling Procedures Samples can be taken from the distillate and the bottom product for analysis: Distillate sampling: i. Drain any remaining liquid in the sampling valve V11. ii. Place a vial below valve V11. iii. Set the reflux divider to total distillate offtake for a few seconds. iv. Open valve V11, collect enough sample and close the valve. v. Switch the reflux divider back to the original setting. Bottom sampling: i. Drain any stagnated liquid above valve V8. ii. Place a vial below valve V8. iii. Open valve V8, collect enough sample and close the valve. Be careful of the hot liquid while collecting a sample. iv. Cool the sample by immersing the vial in cold water. Note: Always re-cap the vials quickly after collecting samples to avoid excessive evaporation of ethanol before analysis. D. Preparation of Calibration Curve Refractive index (RI) readings are used to determine the composition of ethanol-water mixtures in the samples. 1) Prepare a set of mixtures containing ethanol and water within a specified range of composition between pure water and pure ethanol. Refer to the sample table in Appendix A. 2) For each mixture, obtain their refractive index readings using a refractometer. 3) Plot the calibration curve of RI vs. composition for the whole range of mixtures. 4) Examine the calibration curve. Note that a strong relationship exists between the RI and composition of ethanol-water mixtures at low concentrations. However, observe that the curve will flatten at the mid range concentrations and starts to slope downwards at high concentrations. At this range, it is difficult to obtain an accurate value for ethanol composition.

Exp/Distillation Column

CPE554

Universiti Teknologi MARA

E. Composition Analysis of Ethanol in Concentrated Samples Measure the refractive index of a sample and determine its composition from the calibration curve. If the composition value is difficult to be determined accurately due to the calibration curves flat slope, dilute the sample so that a more accurate reading can be obtained. Perform the dilution as follows: 1) Place a 10 mL measuring cylinder on a weighing scale (accurate to 0.01 g) and zero the scale. 2) Using a dropper, transfer 1 to 2 g of sample into the measuring cylinder. Record the sample weight. 3) Add water into the measuring cylinder to dilute the sample. Obtain a total solution weight in the range of 5 to 10 g. Record the solution weight. 4) Ensure that the diluted solution is well mixed before measuring its refractive index (RI). 5) Obtain the diluted solution's composition from the calibration curve. 6) Calculate the actual sample's composition as folows:

7) Use the sample table in Appendix C for data recording and calculation.

EXPERIMENT : Batch Distillation At Total Reflux

OBJECTIVE: To determine the number of theoretical plates at total reflux. PROCEDURES: 1. Perform the general start-up procedures (Section A). 2. Once the distillation column has reached stable condition, record the trays, top and bottom temperature. 3. Collect samples from the distillate and bottom product (Section C). 4. Measure the refractive index for all samples and determine their compositions (Section E).

ANALYSIS & DISCUSSION: 1. Use the sample table in Appendix B for data collection. 2. Using the X-Y equilibrium diagram for ethanol-water system, mark the trays, top and bottom compositions on the diagram and determine the number of theoretical plates in the distillation column using the McCabe-Thiele method.

Exp/Distillation Column

CPE554

Universiti Teknologi MARA

Exp/Distillation Column

CPE554

Universiti Teknologi MARA

Exp/Distillation Column