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Distillation Column Experiment — Reflux Ratio, Tray Efficiency and McCabe-Thiele Method

Aim of the Experiment

To study the operation of a distillation column, to determine tray efficiency using the McCabe-Thiele graphical method, and to study the effect of reflux ratio on product composition and column performance.

Apparatus Required

  • Distillation column (sieve tray or bubble cap column)
  • Reboiler with heater and temperature controller
  • Condenser with cooling water supply
  • Reflux divider / splitter
  • Refractometer or hydrometer (for composition measurement)
  • Thermometers / temperature sensors at each tray
  • Sampling ports at feed, distillate, and bottoms

Theory

Distillation is a separation process based on differences in volatility (boiling points) of components in a liquid mixture. In a distillation column, vapour rises up the column and liquid flows downward. At each tray, vapour and liquid come into contact and approach equilibrium — the more volatile component (MVC) concentrates in the vapour phase.

Reflux Ratio: R = L/D, where L is liquid returned to the column (reflux) and D is distillate product flow.

Operating Line (Rectifying section): y = [R/(R+1)] × x + x_D/(R+1)

McCabe-Thiele Method: Graphical construction on a vapour-liquid equilibrium (VLE) diagram. Theoretical trays are stepped off between the equilibrium curve and operating lines. Tray efficiency = (actual trays) / (theoretical trays needed).

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Murphree Tray Efficiency: E_mv = (y_n − y_{n+1}) / (y*_n − y_{n+1})

Procedure

  1. Charge the reboiler with a known feed mixture (e.g., ethanol-water, 30–40% ethanol by volume).
  2. Switch on the heater. Set the reflux ratio to a known value (e.g., R = 3).
  3. Allow the column to reach steady state (approximately 45–60 minutes). Monitor temperatures at each tray — they should stabilise.
  4. Collect samples from the distillate and bottoms outlets.
  5. Measure compositions (mole fractions) of distillate (x_D) and bottoms (x_B) using a refractometer or calibrated hydrometer.
  6. Draw the McCabe-Thiele diagram: plot VLE curve, rectifying operating line, stripping operating line, and step off theoretical trays.
  7. Calculate overall column efficiency: E_o = N_theoretical / N_actual.
  8. Repeat for a different reflux ratio (e.g., R = 5) and compare distillate composition and efficiency.

Observation Table

ParameterRun 1 (R=3)Run 2 (R=5)
Feed composition x_F (mole fraction)
Distillate composition x_D
Bottoms composition x_B
Reboiler temperature (°C)
Distillate temperature (°C)
Theoretical trays (McCabe-Thiele)
Actual trays
Overall efficiency E_o (%)

Result

Overall tray efficiency at R = 3: E_o = _______%. At R = 5: E_o = _______%. A higher reflux ratio gives purer distillate but reduces column capacity and increases energy consumption. The McCabe-Thiele construction confirms the number of theoretical stages required.

Related: Process Engineering Lab Equipment | Process Engineering Lab Setup Guide | Dissolution Apparatus Experiment | Instruments in Chemistry Lab

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