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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CONTENTS

1 Introduction

2 Experiment 1: Absorption of Ammonia (N H3)

3 Operational Information

4 Thermodynamic Phase-Equilibrium

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

16.1 Gas feed-line rotameters (RTM):

25
. . . . . . . . . . . . . . . . . . . . . . . . . . . . .

25

16.2 Measurements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

26

(N H3 + N2 )

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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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

l The

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

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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EXPERIMENT 1: ABSORPTION OF AMMONIA (N H3 )

Counter-current absorption packed tower

Nomenclature

l Solute:
Raffinate (N2 + NH3)
Vout, yout

Solvent (W)
Lin, xin

l Feed

Ammonia

Carrier Gas: Nitrogen

l Solvent:

Rotameter

(N H3)

Water

(N2)

(W )

Thermodynamic Equilibrium

Ammonia
Sensor

Feed-solvent Phase
(or raffinate phase)

h
N2 + NH3
W

Equilibrium
y = mx*

N2 + NH3
W + NH3

x*

Extract-solvent Phase
(or extract phase)

Vin, yin
Rotameter
Feed (N2 + NH3)

Lout, xout
Extract (W + NH3)

Assumption: Nitrogen is insoluble in

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OPERATIONAL INFORMATION

l Column

available

m Height

of the column :

m Internal
m Type

diameter:

800 mm

100 mm

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

W ) is nonvolatile at the temperature of

are making the assumption that the solvent (

the experimental conditions

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OPERATIONAL INFORMATION

l Continuous
m Two

and dispersed phases

phases form inside the column:

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
m Start
m Set

at 0% ooding

gas ow

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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THERMODYNAMIC PHASE-EQUILIBRIUM

l Some N H3 from the gas phase (Nitrogen + N H3) absorbs into the
N H3) establishing a phase equilibrium after a suciently long time

l The

liquid phase (Water +

mole fraction of

N H3

in the liquid phase at equilibrium

mole fraction of

N H3

in the gas phase at equilibrium

equilibrium mole-fraction

(x)

of absorbed

N H3

is known as the solubility of

N H3

in

water

y
N2 + NH3

Gas Phase
Liquid Phase

W + NH3

x*

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THERMODYNAMIC PHASE-EQUILIBRIUM

l The

solubility of

m The
l It

N H3

in water is high at room temperature and

1 atm

of pressure

solubility increases with pressure and decreases with temperature

x to y , but we are
N H3 and nitrogen)

is possible to derive a relationship relating

of low values of

m Focus:

(use of dilute mixture of

mostly interested in cases

dilute gas-phase regime

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HENRY'S LAW

l At constant T

and at equilibrium, the amount of solute gas that dissolves into the liquid

is proportional to the partial pressure

(yP )

(x)

of the solute gas in the gas phase: i.e,

yP = H(T )x

(1)

y = mx

(2)

or

where

m=
where

H (T )
P

(3)

is the operating pressure of the column and

H (298.15) = 0.885 atm

l Valid
(

only for dilute solutions and when the solute

W)

l Temperature

does not react with the solvent

dependence is given by the van't Ho equation

H (T ) = H T
and for

(N H3)

N H3/water

ref

exp C

1
1
ref
T
T


(4)

solution

C = 3670 K
l Resource:

http://www.henrys-law.org

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GAS DENSITIES

l Standard

Temperature and Pressure

m NIST-STP:

National Institute of Standards and Technology

T = 20 C = 68 F = 293.15 K

m IUIPAC-STP:

P = 1 atm = 1.01325 bar = 14.696 psi

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 )

Air =

where

P
Specific
T
RAir

(5)

is the feed gas pressure and

Specific
RAir
= 286.689 J/ (kg K) = 2.829 103 m3 atm/ (kg K)

m Density

of ammonia gas

N H3

M WN H3
17.031
Air =
Air = 0.587Air
M WAir
29

(6)

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COLBURN'S NTU EQUATION

7.1 Number of transfer units for gas-phase controlled transfer

NOG

mxin yout
A
mx yin

 in
ln
=
1
mx

y
1A
in
out
1
1
A
mxin yin

(7)

and

L0in
A =
mVin0

(8)

where

yout
yin
xin
A
Vin0 = Vin/Across
L0in = Lin/Across
m

solute mole fraction in the ranate

[dimensionless]

solute mole fraction in the feed

[dimensionless]

solute mole fraction in the solvent

[dimensionless]

absorption factor

solvent molar supercial velocity

[dimensionless] 2

lbmole/ min ft2

lbmole/ min ft

equilibrium constant for dilute solution

[dimensionless]

feed molar supercial velocity

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COLBURN'S NTU EQUATION

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

HOG =
lh

(9)

is the height of the packed bed [ft]

7.3 Remarks on the NTU Equation

l Only
l It

h
NOG

(7)

valid for dilute feed streams

is assumed that the solute mole fraction in the solvent is zero, i.e.,

l Number

of transfer units is expressed in terms of concentration in the gas phase

m Solubility
l As

xin = 0

of ammonia in water is high

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

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OVERALL MASS TRANSFER COEFFICIENT

l Overall

mass transfer coecient on a gas-phase basis

Vin
1
=
Vin0
HOGAcross HOG
m Interfacial area per unit volume of packing, a, is normally
transfer coecient (Denition: Ainterf acial = aAcross )
Ky a =

l Mass-transfer

left lumped with the mass

resistance: inverse of the mass-transfer coecient

Resistance =
l Correlation

(10)

1
Ky a

(Solve using least-squares regression)

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

where

m See

(11)

(12)

c4 = ln c1
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


(Ky a)

correlation (Ky a)run
Error =
100%
(Ky a)run

(13)

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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

A=

Slope of operating curve

Slope of equlibrium curve

(L0in/Vin0 )
L0in
=
=
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

A>1
m Hence,

N H3 from
A is met.

the absorption of

the above condition on

mxin yout
mxin yin

the gas phase into the liquid phase occurs only when

l Observations
m When A < 1

desorption

or

m When A = 1

mxin yout
mxin yin

mass transfer occurs from the liquid phase into the gas phase

stripping )
mxin yout
mxin yin

there is no net mass transfer between the gas and liquid phases

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10

INTERPRETATION OF NTU AND HTU

l Number

of transfer units (NTU)

m Depend

on the value of

m Measure
m If

yout

desired for a given

yin

of the diculty of separation

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
m HTU

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

is proportional to the resistance to mass transfer

HOG =
m HTU

1 Vin
Ky a Across

(14)

is small (lower resistance) when

n There
n There

is a high rate of interface mass transfer

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)

tholdup =
tholdup
QW ater
VP ack

VP ack
QW ater

(15)

hold-up time (residence time)

(min)

water (solvent) ow rate

(GPM)

packed volume

(gal)

11.2 Number of hold-ups

Nholdup =
Nholdup
tSS

tSS
tholdup

number of hold-ups

(dimensionless)

time to steady-state

(min)

(16)

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12

SCRUBBING EFFECTIVENESS

l Denition

of Scrubbing Eectiveness

 :=
l Formula

N H3absorption into the liquid solvent

N H3entering via the feed stream

Overall rate of
Rate of

Derivation: Dene

Y =
and use the mass-balance result

Vout =

yout
yin

(18)

1 yin
Vin:
1 yout


 =

(17)

yinVin youtVout
yinVin

1 yin
Vin
yinVin yout
1 yout
=
yinVin

yin (1 yout) yout (1 yin)

yin yout
=
yin (1 yout)
yin (1 yout)
yout
1
1Y
yin
=
=
yout
1 yinY
1 yin
yin

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

n Calculate

yout
yin

Y exp =
n Calculate

m 2. From NTU predictions
Information needed: yin , m, Vin , Lin ,

exp

(19)

1 Y exp
=
1 yinY exp

and

(20)

NOG

Procedure

n Calculate A

and nd the value of

NOG =

by solving (graphically or numerically) from

A
ln
A1

n Calculate
pred =
m 3. Prediction error
n Calculate the prediction

error

1+

1
(A 1)
Y
A

1Y
1 yinY

(21)

(22)

PE
PE =

 pred


exp
exp

100%

(23)

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13

THEORETICAL EXPECTATIONS

l The

mass transfer should increase for larger

l The

mass transfer should more strongly aected by the gas-feed ow rate

solvent ow rate

Lin/Vin

ratios

(Vin)

than by the

(Lin)

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14

MEASUREMENT OF

l BACHARACH

Ammonia

N H3

gas

GAS COMPOSITIONS

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 122F (0

to 50C)

l Accuracy: 10 ppm 10%

from 0 1000 ppm

of reading

l Operating

Humidity: 5 to 90% RH, non-

condensing

l Response

Time:

to

30 seconds,

depend-

ing on tube length and gas concentration

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15

ROTAMETER: WATER FLOW MEASUREMENT

15.1 Liquid solvent rotameter (RTM):

water

l Dwyer

Rate-Master Flowmeter:

Coarse

Fine

Model

RMC

l2

rotameters

(coarse

and

ne

adjust-

ments)

l Measurement
m Coarse:
m Fine:

units

Gallons per Minute (GPM)

Gallons per Hour (GPH)

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ROTAMETER: WATER FLOW MEASUREMENT

15.2 Measurements
l Reading: QRT M,solvent

l For

(graduation mark on the scale)

ne rotameter

Qsolvent(GP H) = QRT M,solvent

l For

coarse rotameter

Qsolvent(GP H) =

l Mass

60 min
QRT M,solvent
1 hr

(24)

(25)

ow rate

Qsolvent(lb/hr) = solventQsolvent(GP H)

(26)

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16

ROTAMETERS: GAS FLOW MEASUREMENTS

16.1 Gas feed-line rotameters (RTM):

Coarse

Fine

(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
Qf eed(SCF H) = RRT M

Pf eed Tref (K)

Pref Tf eed(K)

Qf eed(lb/hr) = fSCF HCF H f eed Qf eed(SCF H)

where the conversion factor

fSCF HCF H

(27)

(28)

is

fSCF HCF H =

Pref Tf eed(K)
Pf eed Tref (K)

(29)

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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
m Take

the

N H3

composition in the feed and ranate stream using the sensor.

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 rotameters 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
l Note

the column at various values of the absorption coecient.

also that at steady state the

N H3

composition in the extract stream is estimated from

the following expression (obtained from a mass balance)

xout =
where

Vout

yinVin youtVout
Lout

(30)

is obtained from yet another mass-balance calculation as

Vout =

1 yin
Vin
1 yout

(31)

l Assumptions
m The N H3/N2

mixture behaves as an ideal-gas mixture

m The

solvent stream contains no absorbed

m The

extract stream contains no absorbed nitrogen

N H3

on inlet to the column

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EXPERIMENTAL DETAILS

l Example

of a data record

m Consider
Run

recording your data in a table

similar

QRT M,f eed QRT M,solvent

to the one shown below

yin

yout

5
..
.

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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 +

Important note:

3.

N H3).

DO NOT turn o the feed gas before turning o the water.

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
l Not

start-up sequence (creates the wrong dispersed phase)

waiting suciently for steady-state conditions

l Experiments
l The

may not have been carried out at isothermal conditions

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

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

l Objective

m Determine

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

state as a function of absorption factor

l Objective

A.

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

m Characterize
n Find

the mass transfer coecient

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
m Plot

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

l Objective
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,

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