Ammonia Gas Absorption

by

Oscar D. Crisalle

Professor

Chemical Engineering Department

University of Florida

crisalle@che.ufl.edu

Revision 12: September 24, 2013

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Ammonia Absorption Rev 08 - 04/15/2013 Page 1
 CONTENTS

1 Introduction 4
2 Experiment 1: Absorption of Ammonia (N H3) 5
3 Operational Information 6
4 Thermodynamic Phase-Equilibrium 9
5 Henry's Law 11
6 Gas Densities 12
7 Colburn's NTU Equation 13
7.1 Number of transfer units for gas-phase controlled transfer . . . . . . . . . . . . . . . . . . . . . . 13
7.2 Height of a transfer unit for gas-phase controlled transfer . . . . . . . . . . . . . . . . . . . . . . . 14
7.3 Remarks on the NTU Equation (7) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

8 Overall Mass Transfer Coecient 15

9 Interpretation of the Absorption Factor 16
10 Interpretation of NTU and HTU 17
11 Characteristics of Flow in the Column 18
11.1 Hold-up time (also called residence time) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
11.2 Number of hold-ups . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18

12 Scrubbing Eectiveness 19
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13 Theoretical Expectations 21
14 Measurement of N H3 Gas Compositions 22
15 Rotameter: Water Flow Measurement 23
15.1 Liquid solvent rotameter (RTM): water . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
15.2 Measurements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24

16 Rotameters: Gas Flow Measurements 25

16.1 Gas feed-line rotameters (RTM): (N H3 + N2 ) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
16.2 Measurements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26

17 Experimental Details 27
18 Experimental Procedures 30
18.1 Start-up and normal-operation procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
18.2 Shut-down procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31

19 Anticipated Experimental Problems 32

20 Objectives 33

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1 INTRODUCTION

l This experiment investigates the properties of gas absorption equipment where a gaseous

solvent mixed with air or Nitrogen is absorbed by dissolution into a water stream

l There are two gas absorption experiments in the Unit Operations lab

Experiment 1 Absorption of ammonia in water

Experiment 2 Absorption of carbon dioxide in water

l The focus of this lab is the Experiment 1 which deals with the absorption of ammonia in

water.

l It is MANDATORY to read the chapter entitled Gas Absorption in reference [3]

before carrying out this experiment.
l Remark: Gas absorption is also referred to as gas scrubbing, or gas washing.

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2 EXPERIMENT 1: ABSORPTION OF AMMONIA (N H3 )

Counter-current absorption packed tower Nomenclature

l Solute: Ammonia (N H3)

Raffinate (N2 + NH3) Solvent (W) l Feed Carrier Gas: Nitrogen (N2)
Vout, yout Lin, xin
l Solvent: Water (W )
Rotameter

Thermodynamic Equilibrium

Feed-solvent Phase
Ammonia h (or raffinate phase)
Sensor
y
N2 + NH3 Equilibrium N2 + NH3

y = mx* W + NH3
W x*

Extract-solvent Phase
(or extract phase)

Vin, yin Rotameter Lout, xout

Feed (N2 + NH3) Extract (W + NH3)
Assumption: Nitrogen is insoluble in W
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3 OPERATIONAL INFORMATION

l Column available

m Height of the column : 800 mm

m Internal diameter: 100 mm
m Type of packing: Standard 6 mm Raschig rings

l Density
m The liquid water stream has a higher density than the N2 + N H3 gas stream. That is why

the liquid stream is fed from the top.

l Insolubility
m We are making the assumption that N2 is insoluble in W. This is only an approximation.

l Nonvolatility
m We are making the assumption that the solvent ( W ) is nonvolatile at the temperature of
the experimental conditions

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OPERATIONAL INFORMATION

l Continuous and dispersed phases

m Two phases form inside the column: a CONTINUOUS phase and a DISPERSED
phase. When a column is started up, it is FIRST lled with ONLY the gas. This denes

the continuous phase. SECOND, the liquid stream is introduced, and it becomes the

dispersed phase.

m Making the gas the continuous phase creates more interfacial area than when the liquid is
the continuous phase (because the gas is constrained to reside in bubbles)

l Flooding by the water phase

m Occurs when the upward force exerted by the gas is sucient to prevent the liquid from

owing downward

m The 100% ooding velocity of the gas stream can be determined for a given inlet liquid

stream ow:

n Set the gas feed ow to a value that oods the column (water level is at the top of the

packing surface)

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OPERATIONAL INFORMATION

l Operation at 0% ooding

m Start gas ow

m Set 100% ooding conditions

m Progressively reduce the gas ow rate until a value where zero ooding (packing base level)
occurs

m Space below packing base must be covered with water to prevent gas escape via the liquid
exit pipe

l In the case of unpacked column

m For 0% ooding, the height of the column at which the inlet of the feed gas stream is

located should be considered as the base level

m For 100% ooding, the height of the column at which the inlet of the water solvent stream
is located should be considered as the top level

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4 THERMODYNAMIC PHASE-EQUILIBRIUM

l Some N H3 from the gas phase (Nitrogen + N H3) absorbs into the liquid phase (Water +

N H3) establishing a phase equilibrium after a suciently long time

x∗ mole fraction of N H3 in the liquid phase at equilibrium

y mole fraction of N H3 in the gas phase at equilibrium

l The equilibrium mole-fraction (x∗) of absorbed N H3 is known as the solubility of N H3 in

water

y
N2 + NH3 P
Gas Phase

W + NH3
Liquid Phase x* T

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THERMODYNAMIC PHASE-EQUILIBRIUM

l The solubility of N H3 in water is high at room temperature and 1 atm of pressure

m The solubility increases with pressure and decreases with temperature

l It is possible to derive a relationship relating x∗ to y , but we are mostly interested in cases

of low values of y (use of dilute mixture of N H3 and nitrogen)

m Focus: dilute gas-phase regime

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5 HENRY'S LAW

l At constant T and at equilibrium, the amount of solute gas that dissolves into the liquid (x∗)
is proportional to the partial pressure (yP ) of the solute gas in the gas phase: i.e,

yP = H(T )x∗ (1)

or

y = mx∗ (2)

where
H (T )
m= (3)
P
where P is the operating pressure of the column and

H (298.15) = 0.885 atm

l Valid only for dilute solutions and when the solute (N H3) does not react with the solvent

( W)
l Temperature dependence is given by the van't Ho equation
  
ref

1 1
H (T ) = H T exp −C − ref (4)
T T
and for N H3/water solution

C = 3670 K
l Resource: http://www.henrys-law.org

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6 GAS DENSITIES

l Standard Temperature and Pressure

m NIST-STP: National Institute of Standards and Technology

T = 20 C = 68 F = 293.15 K P = 1 atm = 1.01325 bar = 14.696 psi

m IUIPAC-STP: International Union of Pure and Applied Chemistry

T = 0 C = 32 = 273.15 K P = 0.9869 atm = 1 bar = 14.504 psi

m Gas rotameter manufactures usually use dierent standards. Refer the instrument manual

for details.

l Density Models
m Density of dry air (model using the specic air constant )
P
ρAir = (5)
Specific
RAir T
where P is the feed gas pressure and
Specific
RAir = 286.689 J/ (kg · K) = 2.829 × 10−3 m3 · atm/ (kg · K)
m Density of ammonia gas
M WN H3 17.031
ρN H3 ≈ ρAir = ρAir = 0.587ρAir (6)
M WAir 29
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7 COLBURN'S NTU EQUATION

7.1 Number of transfer units for gas-phase controlled transfer

mxin − yout
A mx − yin
NOG = ln  in  (7)
1−A 1 mx in − y out
1− 1−
A mxin − yin
and
L0in
A = (8)
mVin0
where

yout solute mole fraction in the ranate [dimensionless]

yin solute mole fraction in the feed [dimensionless]

xin solute mole fraction in the solvent [dimensionless]

A absorption factor
[dimensionless] 2

Vin0 = Vin/Across feed molar supercial velocity
lbmole/ min · ft2

L0in = Lin/Across solvent molar supercial velocity lbmole/ min · ft
m equilibrium constant for dilute solution [dimensionless]

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COLBURN'S NTU EQUATION

7.2 Height of a transfer unit for gas-phase controlled transfer

h
HOG = (9)
NOG
lh is the height of the packed bed [ft]

7.3 Remarks on the NTU Equation (7)

l Only valid for dilute feed streams

l It is assumed that the solute mole fraction in the solvent is zero, i.e., xin = 0
l Number of transfer units is expressed in terms of concentration in the gas phase

m Solubility of ammonia in water is high

l As a result, the dominant resistance to diusion (mass transfer) resides within the gas

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8 OVERALL MASS TRANSFER COEFFICIENT

l Overall mass transfer coecient on a gas-phase basis

Vin 1
Ky a =
= Vin0 (10)
HOGAcross HOG
m Interfacial area per unit volume of packing, a, is normally left lumped with the mass

transfer coecient (Denition: Ainterf acial = aAcross )

l Mass-transfer resistance: inverse of the mass-transfer coecient

1
Resistance = (11)
Ky a
l Correlation (Solve using least-squares regression)

Ky a = c1Lcin2 Vinc3 =⇒ ln (Ky a) = c4 + c2 ln Lin + c3 ln Vin (12)

where c4 = ln c1
m See tutorial on the Excel function LINEST ( Least-squares regression using LINEST in

Excel ) posted in the course web site. You can also use MATLAB or OCTAVE

m Verication of correlation
n Carry out at least one additional experimental run
 
correlation − (Ky a)run
(Ky a) 
Error = 100% (13)
(Ky a)run
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9 INTERPRETATION OF THE ABSORPTION FACTOR

l The Absorption Factor A is dened as the ratio of the local slope of the operating curve

to that of the equilibrium curve

Slope of operating curve (L0in/Vin0 ) L0in

A= = =
Slope of equlibrium curve m mVin0

l For the transfer of N H3 from the gas phase (V ) to the liquid phase (L), the driving force
y − y ∗ should be positive, which implies the operating line should be above the equilibrium
line.

m This is possible when

mxin − yout
A>1−
mxin − yin
m Hence, the absorption of N H3 from the gas phase into the liquid phase occurs only when

the above condition on A is met.

l Observations
mxin − yout
m When A < 1 − mass transfer occurs from the liquid phase into the gas phase
mxin − yin
(desorption or stripping )
mxin − yout
m When A = 1 − there is no net mass transfer between the gas and liquid phases
mxin − yin

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10 INTERPRETATION OF NTU AND HTU

l Number of transfer units (NTU)

m Depend on the value of yout desired for a given yin

m Measure of the diculty of separation

m If a high-level of absorption (separation) is desired, then a larger number of NTUs is

needed

l Height of a transfer units (HTU)

m Depend on the mass transfer coecient and the gas ow rate

m Measure of the separation eectiveness of the packing for the species being absorbed

m HTU is proportional to the resistance to mass transfer

1 Vin
HOG = (14)
Ky a Across
m HTU is small (lower resistance) when

n There is a high rate of interface mass transfer

n There is a large amount of interfacial area (better contact)

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11 CHARACTERISTICS OF FLOW IN THE COLUMN

11.1 Hold-up time (also called residence time)

VP ack
thold−up = (15)
QW ater
thold−up hold-up time (residence time) (min)

QW ater water (solvent) ow rate (GPM)

VP ack packed volume (gal)

11.2 Number of hold-ups

tSS
Nhold−up = (16)
thold−up
Nhold−up number of hold-ups (dimensionless)

tSS time to steady-state (min)

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12 SCRUBBING EFFECTIVENESS

l Denition of Scrubbing Eectiveness

Overall rate of N H3absorption into the liquid solvent

 := (17)
Rate of N H3entering via the feed stream
l Formula Derivation: Dene
yout
Y = (18)
yin
1 − yin
and use the mass-balance result Vout = Vin:
1 − yout
 
1 − yin
yinVin − yout Vin
yinVin − youtVout 1 − yout
 = =
yinVin yinVin
yin (1 − yout) − yout (1 − yin) yin − yout
= =
yin (1 − yout) yin (1 − yout)
yout
1−
yin 1−Y
= yout =
1 − yin 1 − yinY
yin

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 l Calculation
m 1. From experimental data
Information needed: yin and yout

Procedure:

n Calculate
yout
Y exp = (19)
yin
n Calculate
exp 1 − Y exp
 = (20)
1 − yinY exp
m 2. From NTU predictions
Information needed: yin , m, Vin , Lin , and NOG
Procedure

n Calculate A and nd the value of Y by solving (graphically or numerically) from

1
A 1+ (A − 1)
NOG = ln Y (21)
A−1 A
n Calculate
1−Y
pred = (22)
1 − yinY
m 3. Prediction error
n Calculate the prediction error PE
 pred 
 − exp
PE = 100% (23)
exp
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13 THEORETICAL EXPECTATIONS

l The mass transfer should increase for larger Lin/Vin ratios

l The mass transfer should more strongly aected by the gas-feed ow rate (Vin) than by the

solvent ow rate (Lin)

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14 MEASUREMENT OF N H3 GAS COMPOSITIONS

l BACHARACH Ammonia gas monitor:

Model AGMSZ

l Measures ammonia gas in the range of 25

to 10, 000 ppm

l Detector Type: Single pass, non-

dispersive infrared

l Sensitivity: 25 ppm
l Operating Temperature: 32 to 122°F (0

to 50°C)
l Accuracy: ±10 ppm ± 10% of reading

from 0 − 1000 ppm

l Operating Humidity: 5 to 90% RH, non-

condensing
l Response Time: 9 to 30 seconds, depend-

ing on tube length and gas concentration

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15 ROTAMETER: WATER FLOW MEASUREMENT

Coarse Fine
15.1 Liquid solvent rotameter (RTM):
water

l Dwyer Rate-Master Flowmeter: Model

RMC

l2 rotameters (coarse and ne adjust-

ments)

l Measurement units

m Coarse: Gallons per Minute (GPM)

m Fine: Gallons per Hour (GPH)

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ROTAMETER: WATER FLOW MEASUREMENT

15.2 Measurements

l Reading: QRT M,solvent (graduation mark on the scale)

l For ne rotameter

Qsolvent(GP H) = QRT M,solvent (24)

l For coarse rotameter

60 min
Qsolvent(GP H) = QRT M,solvent (25)
1 hr

l Mass ow rate

Qsolvent(lb/hr) = ρsolventQsolvent(GP H) (26)

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16 ROTAMETERS: GAS FLOW MEASUREMENTS

Coarse Fine
16.1 Gas feed-line rotameters (RTM):
(N H3 + N2)

l Dwyer Rate-Master Flowmeter: Model

RMB

l2 rotameters (coarse and ne adjust-

ments)

l Measurement units:  Standard Cubic

Feet per Hour (SCFH)

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ROTAMETERS: GAS FLOW MEASUREMENTS

16.2 Measurements

l Reference (from the instrument manual)

m Tref = 70 F = 21.111 C = 294.261 K

m Pref = 1 atm = 1.01325 bar = 14.696 psi

l Reading: RRT M (oat position on the scale)

s
Pf eed Tref (K)
Qf eed(SCF H) = RRT M (27)
Pref Tf eed(K)

Qf eed(lb/hr) = fSCF H→CF H ρf eed Qf eed(SCF H) (28)

where the conversion factor fSCF H→CF H is

Pref Tf eed(K)
fSCF H→CF H = (29)
Pf eed Tref (K)

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17 EXPERIMENTAL DETAILS

l Because N H3 is highly soluble in water, one must operate at low solvent-to-feed rations

(i.e., low L/V) to prevent complete mass transfer to the liquid (dominant resistance to mass

transfer is in the gas phase)

l Measure the N H3 composition in the feed and ranate stream using the sensor.

m Take repeated measurements to obtain statistical averages.

m Report concentration values at steady state (take great care of ensuring steady state is

attained)

l Measure the volumetric mass ow rates of the the feed and solvent streams using the rotame-
ters and convert the readings to mass and molar ow rates [lbmol/hr].

m Then calculate the corresponding uxes need in Colburn's equation by dividing by the

cross sectional area of the column.

l Determine the ooding velocity of the feed stream for each solvent ow rate considered.

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EXPERIMENTAL DETAILS

l Run the column at various values of the absorption coecient.

l Note also that at steady state the N H3 composition in the extract stream is estimated from

the following expression (obtained from a mass balance)

yinVin − youtVout
xout = (30)
Lout
where Vout is obtained from yet another mass-balance calculation as

1 − yin
Vout = Vin (31)
1 − yout

l Assumptions
m The N H3/N2 mixture behaves as an ideal-gas mixture

m The solvent stream contains no absorbed N H3 on inlet to the column

m The extract stream contains no absorbed nitrogen

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EXPERIMENTAL DETAILS

l Example of a data record

m Consider recording your data in a table similar to the one shown below

Run T QRT M,f eed QRT M,solvent yin yout ∆P ···

..
.

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18 EXPERIMENTAL PROCEDURES

18.1 Start-up and normal-operation procedures

1. Plug the power cable of the N H3 sensor into the outlet.

2. Open the valve for the water outlet (extract) line.

3. Open fully the feed-gas cylinder (N2 + N H3). Set the regulator pressure to the desired

setting. (Note: the pressure should not exceed 40 psi)

4. Adjust the rotameters to allow the desired ow of feed gas ow into the column.

5. Open the water inlet valve and adjust the rotameters to obtain the desired solvent (water)

ow into the column. DO NOT allow water into the column when the feed ow rate is zero,

as water might enter into the feed gas line until it reaches and damages the N H3 sensor.

6. Switch on the dierential pressure gauge to measure the pressure drop across the column.

7. Open the appropriate sensor gas-valves to measure the concentration of N H3 in either the

feed stream or the ranate stream.

8. During operation always maintain the water level at the bottom of the column below the

feed-gas inlet to prevent feed gas escaping the column through the extract-stream opening.

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EXPERIMENTAL PROCEDURES

18.2 Shut-down procedure

1. Turn o the solvent ow into the column by closing the water valve completely.

2. Close completely the valve of the feed-gas cylinder (N2 + N H3).

Important note: DO NOT turn o the feed gas before turning o the water.

3. Wait for the feed-gas and water ow into the column to go to zero on the rotameter

scales; then turn o the rotameters.

(Closing the inlet valves of water and feed gas before turning o the rotameters helps

to release the pressure in the inlet lines in shut-down mode)

4. Switch o the pressure gauge.

5. Unplug the Ammonia sensor from the power outlet.

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19 ANTICIPATED EXPERIMENTAL PROBLEMS

l Incorrect start-up sequence (creates the wrong dispersed phase)

l Not waiting suciently for steady-state conditions

l Experiments may not have been carried out at isothermal conditions

l The feed gas may escape through the extract outlet when a small amount of water level is

not maintained at the extract outlet

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20 OBJECTIVES

NOTE: Address ONLY the objectives identied by the instructor (ignore the rest)

l Objective 1

m Characterize the ooding condition of the column at each liquid ow rate by determining
the ooding gas ow rate. Plot the ooding gas ow rate as a function of (a) liquid ow

rate, (b) the liquid-to-gas molar ow ratios, and (c) the absorption factor A

l Objective 2

m Determine the hold-up time and the number of hold-up times needed to achieve steady-

state as a function of absorption factor A.

l Objective 3

m Characterize the dependence of NTUs and HTUs on the absorption factor A: (a) Plot the

NTU and HTU results as a function of A, (b) Plot the natural logarithm of the NTU and

HTU results as a function of A.

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OBJECTIVES

l Objective 4

m Characterize the mass transfer coecient

n Find a correlation for the mass transfer coecient and verify the correlation using

additional experimental test

n Establish the dependence of the mass transfer coecient on the absorption factor A: (a)
Plot the mass transfer coecient as a function of A, (b) Plot the natural logarithm of

mass transfer coecient as a function of A. Superimpose on these plots the correlation

curve

l Objective 5

m Plot the the scrubbing eectiveness as a function of A as a function of the NTUs.

l Objective 6

m Plot the ranate and the extract compositions as a function of A

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REFERENCES

[1] Hodgman, C. D., Weast R. C., and Selby, S. M., editors, CRC Handbook of Chemistry and
Physic s, 42nd edition. CRC Press, Cleveland Ohio, (1961).
[2] Geankoplis, C. J., Transport Processes and Unit Operations, Third Edition. Prentice-Hall Inc.,
Englewood Clis, NJ (1990). (Chapter 10)

[3] McCabe, W. L., J. C. Smith, and P. Harriet, Unit Operations of Chemical Engineering, Fifth
Edition. McGraw-Hill, Inc., New York, NY (1993). (Chapter 22)

[4] Foust, A. S., L. A. Wenzel, C. V. Clump. L. Maus. and L. B. Anderson, Principles of Unit
Operations. John Wiley & Sons, New York, 1960. page 552.
[5] Onda, K., Takeuchi, H., and Okumoto, Y, Mass transfer coecients between gas and liquid

phases in packed columns, Journal of Chemical Engineering of Japan, Vol 1, pp. 5662 (1968).
[6] Treybal, R. E., Mass Transfer Operations, 2nd. ed., McGraw-Hill, New York (1968).

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