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Exp/Distillation Column
CPE554
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
7) Use the sample table in Appendix C for data recording and calculation.
Exp/Distillation Column
CPE554
Exp/Distillation Column
CPE554
Exp/Distillation Column