Chemical Engineering and Processing 40 (2001) 235 243

www.elsevier.com/locate/cep

Experimental study on multicomponent distillation in packed

columns
Sami Pelkonen a,*, Andrzej Gorak b, Andre Ohligschlager c, Ruth Kaesemann d
b

a
Krupp Uhde GmbH, Friedrich-Uhde-Strasse 15, D-44141 Dortmund, Germany
Uni6ersitat Dortmund, Lehrstuhl Thermische Verfahrenstechnik, D-44221 Dortmund, Germany
c
Axi6a GmbH, Industriepark Hochst, D-65926 Frankfurt-am-Main, Germany
d
Uni6ersitat Dortmund, Lehrstuhl Urnwelttechnik, D-44221 Dortmund, Germany

Received 10 June 1999; received in revised form 24 March 2000; accepted 26 May 2000
Professor Alfons Vogelpohl

Abstract
An extensive set of experimental data on multicomponent distillation with non-ideal systems in structured packed columns is
presented to fill the gap of such data in literature. Experimental composition profiles along the column height obtained by
distillation experiments with nonideal systems, methanol 2-propanol water, methanol acetonitrile water, and acetone
methanol2-propanolwater are reported. The distillation columns and the sampling technique are discussed in detail. An
example how to use these data is shown by comparing the experimental data with simulation results when applying different
mathematical models. 2001 Elsevier Science B.V. All rights reserved.
Keywords: Multicomponent systems; Distillation; Experiment; Structured packings; Simulation models

1. Introduction
The existing experimental distillation data are either
used for the determination of model parameters
(HETPs, VLE-parameters, and mass transfer correlations) or for the validation of the mathematical models.
Most of the experimental data published are concerned
with binary systems and contain compositions measured only at the column top and the bottom of the
column. The problems of using such data for model
validation are:
1. The model parameters or the models verified by
binary mixtures are not necessarily valid for multicomponent systems.
2. The conclusions based only on the measurements at
the top of the column and at the bottom of the
column provide little information about the behaviour inside the column. Such information may
be of essential importance when investigating the

* Corresponding author. Tel.: +49-231-5472424.

E-mail address: pelkonens@kud.thyssenkrupp.com (S. Pelkonen).

distillation of non-ideal mixtures with distillation

boundaries.
The publications known to us illustrating experimental composition profiles along the column height on
multicomponent distillation with structured packed
columns are summarised in Table 1. These experiments
have been used for the investigation of the mass transfer mechanism [15,17], for the steady-state and dynamic
model validation [3,4,8 13,16] and for the model
parameter determination [2]. Recently, Baur et al. [1]
have used experimental data to examine the behaviour
of distillation boundaries in multicomponent azeotropic
mixtures.

2. Set-up of the distillation columns

Fig. 1 illustrates the distillation column used at the
University of Clausthal. The column consists of a reboiler (2), two packed section (3) and a total condenser
(5). The column was equipped with Sulzer BX and
Platte K. Both sections have a diameter of 100 mm and

0255-2701/01/$ - see front matter 2001 Elsevier Science B.V. All rights reserved.
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S. Pelkonen et al. / Chemical Engineering and Processing 40 (2001) 235243

236

Table 1
Experimental multicomponent distillation data on structured packings with compositions along the column height
Source

Packing

Column
dimensions D, h

Column operation

Test systems

[3,4,10,11]

70 mm, 2.5 m

[8]

Sulzer DX,
Sulzer BX
Sulzer CY

100 mm, 0.8 m

20 mbar, Partial reflux,

dynamic operation
1000 mbar, Total reflux

Six-component-fatty-alcohol
mixtures
Methanol/2-propanol/water

[9]

Sulzer BX

100 mm, 0.8 m

1000 mbar, Total reflux

[2]

Sulzer BX

10 mbar, Partial reflux

[17]

RomboPak 6M

70 mm, 1 m,
70 mm, 2 m
150 mm, 2.2 m

950 mbar, Total reflux

[12]

Mitsubishi
MC-250T
Montzpak
A3-500
Rombopak 6M

210 mm, 3 m

1000 mbar, Partial reflux

100 mm, 3 m

1000 mbar, Total reflux

100 mm, 3 m

1000 mbar, Partial reflux,

dynamic operation

[13]
[16]

Composition data

Five compositions along the

column height
Ten compositions along the
column height
Methanol/2-propanol/water/ Ten compositions along the
acetone
column height
Ternary fatty alcohol
Five compositions along the
mixtures
column height
Cyclohexane/toluene/chloro- 11 compositions along the
benzene
column height
methanol/acetonitrile/water
Methanol/ethanol/water
Six compositions along the
column height
Methanol/acetonitrile/water 16 compositions along the
column height
Extractive distillation of
16 compositions along the
acetone/methanol with
column height
water

Fig. 1. Flow-diagram of the pilot plant column constructed at the University of Clausthal.

S. Pelkonen et al. / Chemical Engineering and Processing 40 (2001) 235243

Fig. 2. P&I-diagram of the pilot plant column constructed at the University of Dortmund.

237

S. Pelkonen et al. / Chemical Engineering and Processing 40 (2001) 235243

238

Fig. 3. Metal gauze wire packing Montzpak A3-500 with a liquid

collector basin.

Fig. 4. Device used for measurement of the liquid maldistribution

below the lowest packing section.

The liquid is taken out of the column with a teflon tube

and led into a sampling flask. Additional samples are

taken from the reflux and the condensate at the top of

the column. When the column is operated at finite
reflux the distillate is introduced into the reboiler so
that no additional feed is needed. The reflux is fed back
into the column at its boiling point. The volume stream
is measured with a rotameter (7) and a damming basin
(8).
Fig. 2 shows the column set-up used at the University
of Dortmund. The column has been constructed following the criteria of Goedecke et al [6] and has an inner
diameter of 100 mm. In the experiments the gauze wire
packing Montzpak A3-500 and the lamella packing
type Rombopak 6M from Kuhni AG were investigated.
The effective packing height amounts to 3 m divided
into three sections, each 1 m high. The liquid flowing
down the column is collected between each section and
is redistributed by means of liquid distributors from
Julius Montz GmbH. The column is made of glass
surrounded by an electrically heated insulation jacket in
order to reduce heat losses. The feed(s), which may be
pre-heated, can be introduced into the column at the
packing heights of 1 or 2 m. A thermosyphon reboiler
and a total condenser with a reflux divider are used. A
condensate accumulator is provided in order to guarantee a steady reflux flow. The operational variables such
as column top pressure, pressure drop, column temperature profile, feed flow rates, feed temperature, reboiler
heat duty, distillate mass stream and reflux ratio are
measured or controlled by a process control unit. The
distillate mass flow rate is measured by a coriolis massflow meter. Composition and temperature can be measured at 18 different locations that are placed at the
same column height. Small stainless steel collector
basins are installed directly into the packing for liquid
sampling (Fig. 3). The collector basins are placed at the
heights of 0.1, 0.5 and 0.9 m in each packing section.
The liquid samples are taken with a special syringe out
of the packing. Samples are also taken above and below
the packing sections from the liquid collectors, and the
feed, reflux and product streams.

3. Accomplishment of the experiments

The experiments at the University of Clausthal and
at the University of Dortmund were conducted in simi-

Table 2
Mixtures, packings and column dimensions used in the experiments
Source

[7]

[14]

[14]

Mixture
Packing
Column diameter (mm)
Packing height (m)

Methanol/2-propanol/ water
Sulzer BX, Platte K
100
1.79

Methanol/acetonitrile/water
Montzpak A3-500
100
3

Acetone/methanol/2-propanol/water
Rombopak 6M
100
3

S. Pelkonen et al. / Chemical Engineering and Processing 40 (2001) 235243

239

Table 3
Experimental results for the ternary experiments with methanol2propanolwatera

Table 3 (Continued)
h

XMeOH

XIP

XMeOH

XIP

MIW 9
0
0.1
0.205
0.320
0.405
0.505
0.705
0.805
0.810
0.942
1.055
1.168
1.281
1.413
1.526
1.790
TTop
LTop
pTop

0.0377
0.0573
0.1120
0.1259
0.1683
0.2153
0.4229
0.4610
0.4870
0.4987
0.5762
0.5766
0.6234
0.6329
0.6507
0.8175
55.47
43.83
960

0.5156
0.5827
0.5889
0.5827
0.5608
0.5326
0.3952
0.3749
0.3576
0.3483
0.2982
0.2960
0.2652
0.2613
0.2504
0.1357

1.281
1.413
1.526
1.790
TTop
LTop
pTop

0.9625
0.9694
0.9734
0.9799
54.55
43.25
960

0.0243
0.0237
0.0199
0.0146

MIW 10
0.1
0.205
0.320
0.405
0.505
0.605
0.705
0.805
0.905
1.795
TTop
LTop
pTop

0.0566
0.1304
0.1499
0.1998
0.2365
0.3273
0.8591
55.70
45.59
960

0.5835
0.5701
0.5616
0.5339
0.4958
0.4533
0.1097

MIW 13
0
0.1
0.205
0.320
0.405
0.505
0.605
0.705
0.805
0.810
0.942
1.055
1.168
1.281
1.413
1.526
1.790
TTop
LTop
pTop

0.1777
0.3055
0.3758
0.4589
0.5352
0.6551
0.7892
0.8152
0.8468
0.8508
0.8539
0.8542
0.8818
0.9072
0.9052
0.9475
53.62
42.91
960

0.4786
0.4447
0.4087
0.3595
0.3136
0.2387
0.1483
0.1370
0.1131
0.1127
0.1116
0.1084
0.0917
0.0709
0.0704
0.0402

MIW 11
0.1
0.205
0.320
0.405
0.505
0.605
0.705
0.805
1.324
1.795
TTop
LTop
pTop

0.0114
0.0442
0.0522
0.0923
0.1378
0.1651
0.2046
0.2590
0.4304
0.5508
51.05
55.86
960

0.6093
0.6302
0.6320
0.6100
0.5869
0.5674
0.5376
0.5110
0.3956
0.3169

MIW 14
0
0.1
0.205
0.320
0.405
0.505
0.605
0.705
0.805
0.810
0.942
1.055
1.168
1.281
1.413
1.526
1.790
TTop
LTop
pTop

0.0585
0.0911
0.1722
0.1986
0.2577
0.3279
0.3904
0.5521
0.6424
0.6637
0.6693
0.7442
0.7447
0.8033
0.8076
0.8403
0.9245
53.38
38.98
960

0.4558
0.5507
0.5357
0.5279
0.4884
0.4534
0.4412
0.3078
0.2560
0.2382
0.2238
0.1854
0.1831
0.1445
0.1430
0.1157
0.0595

MIW 12
0
0.1
0.205
0.320
0.405
0.505
0.605
0.810
0.942
1.055
1.168

0.2199
0.2968
0.4986
0.5694
0.6247
0.7249
0.8610
0.9023
0.9244
0.9304
0.9590

0.3704
0.4099
0.3204
0.2813
0.2492
0.1787
0.0990
0.0735
0.0554
0.0499
0.0316

MIW 15
0
0.1
0.205
0.320
0.405
0.505
0.605
0.705
0.805
0.810
0.942
1.055

0.0580
0.0779
0.1342
0.1660
0.1860
0.2803
0.3595
0.4885
0.5864
0.5934
0.5942
0.6812

0.4748
0.5610
0.5621
0.5509
0.5429
0.4863
0.4366
0.3513
0.2865
0.2862
0.2928
0.2283

S. Pelkonen et al. / Chemical Engineering and Processing 40 (2001) 235243

240
Table
3 (Continued)
.
h

XMeOH

XIP

1.168
1.281
1.413
1.526
1.790
TTop
LTop
pTop

0.6877
0.7451
0.7602
0.7817
0.8910
54.08
40.31
960

0.2222
0.1825
0.1740
0.1593
0.0825

The packing height 0 m corresponds to the sampling place below

the lowest packing section.

lar way. The column was first filled with the mixture
under investigation. The steady-state composition profiles at total reflux experiments are very sensitive to the
initial composition of the mixture in the reboiler. To
obtain a composition profile that undergoes major
changes in the column the composition profile was
shifted to a preferred direction after having reached the
steady-state by adding the component(s) in too less
extent. After obtaining a desired composition profile a
set of experiments were carried out at total reflux and
at atmospheric pressure by varying the reboiler heat
duty.
The temperature profile along the column height was
observed and stored in a process control unit. After
having reached a constant temperature profile 60120
min were needed to reach a steady-state operation of
the column. This is important due to the possibly flat
temperature changes in spite of large composition variations. Before sampling the temperature profile, the
column top pressure and the pressure drop were measured and stored. After sampling the volume streams at
the top of the column and below the packing were
measured.
The measured streams were compared with those
obtained from the energy balances around the condenser and the reboiler, so that the heat losses from the
column could be calculated. The compositions of the
samples were analysed with a gas chromatograph both
at the University of Clausthal and at the University of
Dortmund. The water content was determined with
TCD and the organic substances with FID.
The experiments are performed in such a way that
the errors caused by heat losses (insulation), extra heat
input (column wall temperature control) or unsteadystate behaviour can be ignored. The volume and surface
area of the collector basins installed directly into the
packing was kept at its minimum in order to prevent a
disturbance of plug flow. The technique was tested in
laboratory with water/air and no disturbance of plug
flow caused by the collector basins could be noticed.
Since maldistribution is present in every packed distillation column, its influence was investigated with a device

Table 4
Experimental results for the ternary experiments with methanolacetonitrilewatera
H

XMeOH

XACN

MAW 1
Cond.
2
1.9
1.5
1.1
1
0.9
0
TTop
VL(Top)
pTop

0.923
0.995
0.997
1
0.833
0.325
0.053
0
54
0.009
1001

0.077
0.005
0.003
5E-04
0
0
0
0

MAW 2
Cond.
2.5
2.1
2
1.9
1.5
1.1
TTop
VL(Top)
pTop

0.922
0.972
0.96
0.942
0.893
0.062
0
57
0.009
999

0.078
0.028
0.006
0.004
0.002
0
0

MAW 3
Cond.
2
1.9
1.5
1.1
1
0.9
0
TTop
VL(Top)
pTop

0.807
0.72
0.66
0.178
0.004
0.002
0
0
52
0.01
1000

0.193
0.28
0.308
0.618
0.729
0.734
0.736
0.032

MAW 4
Cond.
3
2.9
2.5
2.1
2
1.9
TTop
VL(Top)
pTop

0.789
0.791
0.773
0.493
0.025
0.008
0
52
0.008
1021

0.21
0.209
0.227
0.407
0.42
0.276
0.01

MAW 5
Cond.
2.5
2.1
2
1.9
1.5
1.1
TTop
VL(Top)
pTop

0.759
0.766
0.61
0.467
0.255
3E-04
0.017
51
0.01
1021

0.241
0.229
0.337
0.421
0.492
0.01
0.005

MAW 6

S. Pelkonen et al. / Chemical Engineering and Processing 40 (2001) 235243

Table 4 (Continued)
H

XMeOH

XACN

Cond.
2.1
2
1.9
1.5
1.1
TTop
VL(Top)
pTop

0.823
0.773
0.743
0.726
0.349
0
50
0.007
1019

0.16
0.214
0.238
0.249
0.475
0

MAW 7
Cond.
2
1.1
1
0.9
0.5
TTop
VL(Top)
pTop

0.838
0.81
0.77
0.747
0.727
0.108
50
0.01
1026

0.162
0.181
0.207
0.217
0.221
0.027

a
The packing height 0 m corresponds to the sampling place below
the lowest packing section.

illustrated in Fig. 4 installed below the lowest packing

section. The differences in the measured volume flow
rates and the compositions in the six cross sectional slices
were found to be negligible. The maximal relative error
of the composition analysis with the GC was measured
to be 2% and that of the molar liquid load 10%.

241

number of theoretical stages for the equilibrium stage

model, the mass transfer correlations for the equal
diffusivity model and the non-equilibrium stage model
were determined from distillation experiments with a
binary ideally behaving system chloro-/ethlybenzene [14].
In the simulations the activity coefficients were calculated
with the UNIQUAC-model with parameter values obtained on the basis of binary VLE-experiments [5]. The
system acetone methanol 2-propanol water exhibits a
distillation boundary due to an azeotrope between 2propanol and water. The experimental composition in
the liquid distributor at the column height of 2 m was
fixed in the simulations. This composition point was
chosen because the liquid phase is fully mixed (no
maldistribution) and because the composition of 2propanol and water are close to the distillation boundary.
The results show, that the composition profiles end up
to completely different reboiler products depending on
which model is applied: the non-equilibrium model
showing a quite good accordance to the experiment,
whereas the equilibrium stage and equal diffusivity
model predict that the reboiler is filled with 2-propanol.
This result caused us to investigate the theory of distillation boundaries more closely. We found out that the
diffusional interactions between the components need to
be considered when dealing with mixtures exhibiting
distillation boundaries [15]. This result has been recently
validated by Baur et al. [1].

6. Conclusions
4. Listing of experimental data
The parameters that were constant in the experiments
are listed in Table 2. The experimental composition
profiles, column pressure as well as reflux flow rates and
temperatures are summarised in Tables 3 5 for
methanol 2-propanol water, methanol acetonitrile
water and acetone methanol 2-propanol water. The
pressure drop over the column height is not reported
because of its insignificant influence on the composition
profiles in the conditions of the experiments.

The essential content of this paper is a listing of

experimental composition profiles obtained with multicomponent non-ideal systems, in structured packed
columns, at total reflux operation of the column and at
atmospheric pressure. Also valuable technical information is provided for construction of pilot scale distillation
columns. The authors recommend the composition data
to be used for the investigation of the phase equilibria,
mass transfer effects and behaviour of distillation
boundaries.

5. Example: simulation versus experiment

7. Notation

The following example shows how important such

data as presented in this paper may be when investigating
the behaviour inside a distillation column. As an example
Fig. 5 shows the composition profiles along the column
height for each component for an experiment with
acetone methanol 2-propanol water, AMIW3 in
Table 5. The simulated composition profiles with equilibrium stage model [18], equal diffusivity model [17] and
non-equilibrium stage model [19] are presented, too. The

AC
ACN
D
h
IP
LTop

acetone
acetontirile
column diameter, (mm)
packing height, (m)
2-propanol (isopropanol)
liquid molar flux at the column top, (mol/
m2 s)
MeOH methanol
pTop
pressure at the column top, (mbar)

S. Pelkonen et al. / Chemical Engineering and Processing 40 (2001) 235243

242

Table 5
Experimental result for the quaternary experiments with acetonemethanol2-propanolwatera
AMIW1

Cond.
3
2.9
2.5
2.1
2
1.9
1.5
1.1
1
0.9
0.5
0.1
0
TTop
LTop
pTop
a

AMIW2

AMIW3

AMIW4

XAC

XMeOH

XW

XAC

XMeOH

XW

XAC

XMeOH

XW

XAC

XMeOH

XW

0.6255
0.6255
0.5937
0.4384
0.1787
0.1240
0.0927
0.0246
0
0
0
0
0
0
47
16.5
1013

0.3745
0.3745
0.4062
0.5428
0.7338
0.7531
0.7493
0.6241
0.3798
0.2951
0.2340
0.1340
0
0

0.0078
0.0073
0.0083
0.0104
0.0310
0.0423
0.0549
0.1095
0.2380
0.2650
0.2835
0.4925
0.9963
1.0000

0.5350
0.5231
0.4665
0.2445
0.0652
0.0398
0.0310
0.0084
0
0
0
0
0
0
55.8
40.7
1017

0.4164
0.4249
0.4567
0.5444
0.4705
0.4212
0.3952
0.2551
0.1459
0.1105
0.0787
0.0391
0
0

0.0198
0.0182
0.0238
0.0612
0.1321
0.1596
0.1602
0.2062
0.3042
0.3239
0.3529
0.4898
0.9963
1.0000

0.5215
0.5171
0.4598
0.2185
0.0572
0.0360
0.0261
0.0079
0
0
0
0
0
0
55.9
36.9
1018

0.4182
0.4208
0.4509
0.5290
0.4341
0.3874
0.3574
0.2339
0.1281
0.0969
0.0708
0.0381
0
0

0.0197
0.0201
0.0262
0.0725
0.1417
0.1655
0.1771
0.2120
0.2988
0.3118
0.3231
0.3582
0.5994
0.9831

0.5689
0.5646
0.5267
0.3363
0.1034
0.0648
0.0434
0.0104
0
0
0
0
0
0
52.8
24.2
1018

0.4122
0.4158
0.4452
0.5743
0.6127
0.5733
0.5289
0.3497
0.2003
0.1540
0.1147
0.0611
0.0243
0

0.0137
0.0097
0.0124
0.0290
0.0854
0.1127
0.1303
0.1823
0.2826
0.2969
0.3125
0.3339
0.5235
0.9261

The packing height 0 m corresponds to the sampling place below the lowest packing section.

Fig. 5. Experiment with acetone/methanol/2-propanol/water at total reflux operation of the column. Presented are the simulated composition
profiles with non-equilibrium stage model (thick dashed line), equal diffusivity model (thin dashed line) and equilibrium stage model (full line).
The circles indicate the measured compositions.

S. Pelkonen et al. / Chemical Engineering and Processing 40 (2001) 235243

TTop
VL(Top)
W
x

temperature of the reflux stream at the

column top, (C)
liquid volume flow rate at the column top,
(l/s)
water
mole fraction ()

References
[1] R. Baur, R. Taylor, R. Krishna, J.A. Copati, Influence of mass
transfer in distillation of mixtures with a distillation boundary,
Trans. I. Chem. E. Part. A. 77 (1999) 561565.
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