Exp.

G notes

Fractional Distillation, 30Aug2004

page 1

Prelab: provide only for 1-propanol, 1-butanol, and methanol Properties

1-propanol M.W. 60.10 M.P. -127o B.P. 970 Den. 0.804 Sol. (> 10%) H2O, EtOH Hazard
3 1 0

1-butanol

74.12

-900

117.70

0.810

EtOH
1

3 0

methanol

32.04

-98

64.6

0.791

Water, ethanol

3 1 0

1. do not plug mantle directly electric outlet, use controller 2. Use 40/60 mol percent 1-propanol/1-butanol (no cyclohexane or toluene) less toxic 3. Set up fractional distillation (OP27) 4. Set heat at highest level to start, insulate distillation column with glass wool after boiling begins to save time 5. not too fast or slow, distillation should take about 30 min 6. turn back down to 60-80% when vapor starts up column, collect first sample then adjust heat as needed 7. 40/60 solution is standard 8. write procedure during distillation not when finished you may split page, left side procedure, right side table (no scratch paper)

Additional material for Postlab Report

1. Retention times 2. C and XP,v (mole fraction of propanol vapor), and XB,v (mole fraction of butanol vapor).

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3. table with area of propanol (AP), area of butanol (AB), AP/AB, R, XP (mole fraction of propanol), and XB (mole fraction of butanol). sample standard 1 AP AB AP/AB R XP XB 4. example of each calculation. 5. plot of boiling point versus volume 6. calculate HETP 7. copy of chromatograms

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Fractional Distillation, 30Aug2004

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Calculation of Theoretical plates from mole fractions 1. theoretical plate result of simple distillation 2. each distillation (plate) creates vapor more rich in more volatile component 3. column can have several theoretical plates 4. n is total theoretical plates in apparatus 5. n-1 is total theoretical plates of column 6. determine n from mole fraction (X) of components Use complete equation on OP 27.
log n= X P ,v X log B ,v X P ,l X B ,l log

is the volatility ratio = 1.49

XP = nP n p + nB XB = nB n p + nB

nP = moles of propanol, nB = moles of butanol XP,v and XB,v = mole fractions in the vapor at the top of the column, XP,l and XB,l = mole fractions in the pot For this experiment XP,v and XB,v are obtained from first fraction, XP,l and XB,l are obtained from original mixture Calculation of mole fractions from GC data

AP = area of propanol under peak, AB = area of butanol under peak

(AP/nP)std = (AP/nP)sample and (AB/nB)std = (AB/nB)sample (AP/nP)std/(AB/nB)std = (AP/nP)sample /(AB/nB)sample (nP/nB)sample = R = (AP/AB)sample*(AB/nB)std/(AP/nP)std = (AP/AB)sample*(AB/AP)std*(nP/nB)std

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Fractional Distillation, 30Aug2004

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Let C = (AB/AP)std*(nP/nB)std = a calibration factor from standard Then R = (AP/AB)sample*C (mole ratio) = (area ratio of sample)*(calibration factor) R can be used to calculate mole fractions XP and XB
nP n p + nB nP XP / XB = = =R nB nB n p + nB

XP + XB = 1, XB = 1 - XP
R = XP / XB = R RX P = X P R = X P + RX P R = X P (1 + R ) XP 1 XP
log n= X P ,v X log B ,v X P ,l X B ,l log

R (1 X P ) = X P

XP = XB

R 1+R R =1 1+R

HETP =

length of column packing n 1