Hexane Adsorption Progress Report 2

Curty Pinheiro
Word Count: 2109

Samuel Allen

Sean Curtin
11/5/15

Introduction
Gas adsorption is a process in which a fluid phase stream is passed over a
solid phase with the intent of selectively depositing one or more components of the
fluid phase onto the solid phase. In most commercial adsorption processes a
stationary solid (adsorbent) is packed into a column and the fluid is passed through
the packed column until the solid phase is saturated with adsorbed material
(adsorbate). This process can be used for purifying air or other gas phases, such as
separating two different gases, products of a chemical reaction, where only one has
commercial value.
The packed bed then undergoes a regeneration process where adsorbate free
fluid is passed over the adsorbent at high temperature and flow rate which
encourages desorption of the material into the fluid and prepares the adsorbent
packed bed to adsorb more material. During an adsorption column process all of the
adsorption takes place in a relatively narrow region called the mass transfer zone.
As time elapses and more fluid as been put through the column the adsorbent
in contact with the adsorbate reaches saturation and the mass transfer zone
migrates from the fluid inlet towards the fluid outlet while the concentration of the
adsorbate in the fluid outlet is maintained at a value close to zero. At a time known
as the break point the concentration of adsorbate in the outlet fluid begins to rise as
the mass transfer zone closes in on the end of the column, until equilibrium.
Other important parameters for an adsorption column include the total
capacity and the usable capacity of the packed bed as well as their time equivalents.
The stoichiometric capacity is defined as the amount of adsorbate that can be
adsorbed if the entire bed comes into equilibrium with the feed stream while the
usable capacity is the amount of adsorbate that can be adsorbed before the break
point is reached.

These quantities can then be used to determine information about the usage
of the bed including fraction of the bed used and length of unused bed. In this
experiment an air stream containing hexane vapor was passed through a column
packed with activated carbon to remove the hexane vapors by adsorption.
The goals of the experiment are to determine the effects of flow rate and
temperature on the mass transfer zone, breakthrough time, time equivalent to
stoichiometric capacity, time equivalent to usable capacity, fraction of total capacity
used, and stoichiometric capacity. A thorough error analysis will be performed on
the data collected and the experimental results will be compared to literature
values.
Work Completed
The first lab session data had to be excluded due to be wrongly collected. In
this second lab session, the temperature was kept approximately constant at 65F,
with variations during time due to the exothermic process of absorption. Three
different air flow rates were used in the runs, 1 SCFH, 3 SCFH, and 5 SCFH.
A mixture of hot and cold tap water was run through the jacket surrounding
the column in order to control the temperature during each trial. An air flow rate
was selected and the air was passed through two hexane bubblers in series to
introduce hexane vapor into the air stream. The gas was then sampled three times
using the thermal conduction gas chromatography unit to determine the inlet
hexane concentration.
A program called Microlab was used to plot the output voltage of the gas
chromatography unit against time elapsed. The valve was then flipped allowing the
air/hexane mixture to flow through the packed column. As the valve was flipped the
Microlab data collection was started and every 20-30 seconds the gas
chromatography valve was opened allowing for the determination of the effluent
hexane concentration.
Samples were taken until the effluent readings were maintained at a
consistent hexane concentration, which indicated that adsorption column saturation

had occurred. After saturation was reached the column was purged by running a
high flow rate of hexane free air through the activated carbon at a high temperature
in order to encourage desorption of the hexane.
By the data collected, we expect to understand the effects of different flow
rates at the same temperature over our dependent variables.
Key Equations
As seen in Geankoplis [1], the equations below, found in section 12.3, are the
main equations for comprehension and calculation of a packed column:
Time equivalent to stoichiometric capacity, the time would take to get the
packed column in equilibrium, i.e. no longer absorb hexane from air in our
experiment:

(1)

= 0 (1 )
0

Time equivalent to usable capacity, time for breakthrough, when mass

transfer zone reaches the top of the column:

(2)

= 0 (1 )
0

Fraction of total capacity used:

=

(3)

Mass transfer zone/unused bed height:

(4)

= (1 )

Bed height for breakthrough/usable capacity:

=

(5)

Total/stoichiometric capacity:
(6)

= +

Besides these equations, which calculates all parameters needed for a packed
column, we have the trapezoidal rule for numerical integration, which is used to
calculate /0 given any experimental data during time:

(1 )+(2 )

2
1 () (2 1 ) [

(7)

So, from equations 1 to 6, we have defined our dependent variables. We

define as our independent variables the Hexane contaminated air flow rate and
the temperature inside the packed column, both to be analyzed in order to
understand how they change our dependent variables.
Sample Calculations
For the example 12.3-1 of Geankoplis text book, we are able to calculate the
total capacity of the given adsorption column by its experimental data:
Table 1. Calculations made in excel for example 12.3-1.
Time [h]
0.0
3.0
3.5
4.0
4.5
5.0
5.5
6.0
6.2
6.5
6.8

C/Co
0.000
0.000
0.002
0.030
0.155
0.396
0.658
0.903
0.933
0.975
0.993

(1-C/Co)
1.000
1.000
0.998
0.970
0.845
0.604
0.342
0.097
0.067
0.025
0.007

Area
3
0.4995
0.492
0.45375
0.36225
0.2365
0.10975
0.0164
0.0138
0.0048
5.18875

By using the trapezoidal rule, we find time equivalent to total capacity:

= (1
0

) = 5.18
0

Breakthrough time is found to be 3.65h, when = 0.01, by interpolation,

0

which gives us the time equivalent to usable capacity:

3.65

(1

3.65

) = (1 0.01) 3.65
0
0

The fraction of total capacity used to the break point:

3.65
=
= 0.704
5.18
Given the bed lengh to be 14cm, we calculate:
= (1
=

) = (1 0.704) 14 = 4.144

= 0.704 14 = 9.856

Data Analysis
The temperature was kept approximately constant, but due to variations
during the process, all temperature was recorded and the average temperature was
68.45F.
For this temperature, at different flow rates for hexane-contaminated air,
several graphs were plot, showing the comparison between the air coming out from
the column, after the absorption, and the air coming into the column.
This comparison was made by the mass fraction of hexane in air, bypassing
the column before and after the process to check variations in this fraction, and
checking the fraction in outlet air during time.

100%

C/Co

80%
60%
40%

20%
0%
0

500

1000
Time (s)

1500

2000

Figure 1. This graph shows /0 during time for a flow rate of 1.0 SCFH at 68.45F.
Mass fraction was 37.08% before and 35.04% after the experiment, giving
the average of 36.06% in mass.
Breakthrough time was estimated between as 908.1s by interpolation, and
the total time was estimated as 2166.2s by numeric integration.
This shows the fraction of total capacity used to be 41.9%.

100%

C/Co

80%
60%
40%
20%
0%
0

100 200 300 400 500 600 700 800 900 1000
Time (s)

Figure 2. This graph shows /0 during time for a flow rate of 3.0 SCFH at 68.45F.
Mass fraction was 34.73% before and 32.18% after the experiment, giving
the average of 33.45% in mass.
Breakthrough time was estimated between as 193.3s by interpolation, and
the total time was estimated as 954.1s by numeric integration.
This shows the fraction of total capacity used to be 20.3%.
100,00%

C/Co

80,00%
60,00%
40,00%
20,00%
0,00%

100

200

300
400
Time (s)

500

600

700

Figure 3. This graph shows /0 during time for a flow rate of 5.0 SCFH at 68.45F.
Mass fraction was 36.92% before and 30.30% after the experiment, giving
the average of 33.61% in mass.
Breakthrough time was estimated between as 90.7s by interpolation, and the
total time was estimated as 671.9s by numeric integration.
This shows the fraction of total capacity used to be 13.5%.

During the experiment, a computer was used to collect data from the gas
chromatography device, recording the electrical impulse during time. These
electrical signals generated a graph, from which it is possible to calculate the area
below the curve using trapezoidal method and, by comparing the area of each peak,
air and hexane, with the total area of both peaks for each measurement, the mass
fraction of hexane in air during time can be calculated.
The difference of mass fraction before and after each run is explained by the
decrease in volume of liquid hexane inside the bubblers, which decreases surface
area and mass transfer coefficient, leading to lower concentrations of hexane in air.
The higher the flow rate, the faster the mass transfer coefficient decreases.
As seen in the graphs, breakthrough time and time until saturation were
different as expected, as a higher flow rate will get the packed bed reached
equilibrium in less time, with a higher concentration of hexane due to a higher mass
transfer coefficient, even its value decreases faster than in a lower flow rate.
An increase in air flow rate will decrease breakthrough time and total time,
but it also decreases the fraction of total capacity of the column used, showing that a
low flow rate would increase the usage of the column with a longer breakthrough
and total time.
Preliminary Design Problem Solution
An activated carbon bed is used to control an air stream with a flow rate of
20 m3 hr-1 at 25C and 1 atm pressure. The air contains 4.6 g m -3 of n-hexane.
Assuming that the working adsorption capacity of the bed is 40% of the working
capacity of the experimental setup, determine the working adsorption capacity of
the carbon, the physical dimensions of the activated carbon bed and the mass of the
activated carbon in the bed.
The first step in solving the design problem will be to equate the Reynolds
numbers of the experimental setup and the design problem setup in order to
calculate the diameter of the theoretical column. This is because experimental data
will be used to determine column parameters for the design solution so the two
columns should be in the same flow regime.

Given that the capacity to volume ratio of each column segment remains constant,
the volume/height of the column will be calculated using the following ratio:

=

Where A is the area of the breakthrough curve for each designated section. This
ratio holds true because the size of the mass transfer zone remains constant through
throughout the process. The capacities of each section of the column are calculated
by:

=
0

= (1

)
0

The Volume of the column up to the breakpoint can be calculated as:

2
=
4

The volume of the remaining column can be calculated as:

(1 )
2

0
][
= [
]

4

0
The total column volume is equal to the sum of the breakthrough point
volume and the remainder volume:
= 1 + 2
Once the total volume of the column is known the previously calculated
column diameter can be used to find the total column height.
=

2
4

Given that physical properties of the air stream (density and viscosity) do not
change the velocity of the design problem can be calculated using
and the mass flow rate of hexane in the air stream can then be calculated by:

=

Where is the mass flow rate of hexane in the

experimental column, and is the mass flow rate of hexane in the
column of the design problem. The mass of hexane in the used section of the bed can
be expressed as:
=
The following formula can be used to calculate the mass of both the experimental
and design problem carbon masses:
=

Given that the working adsorption capacity of the bed is 40% of the working
capacity of the experimental setup the following equation will be used to determine
the working adsorption capacity:


[
]
=
0.4


Next Steps
During next week lab session data will be collected to determine the effect of
temperature on breakthrough time, mass transfer zone, time equivalent to
stoichiometric capacity, time equivalent to usable capacity, stoichiometric capacity,
and fraction of unused bed. This will be accomplished by testing the same flow rates
that were tested during the first two weeks of lab (1 SCFH, 3 SCFH, and 5 SCFH) at a
temperature warmer than 68.45F. The desired temperature will be reached by
using an appropriate flow rate of hot and cold tap water streams through the jacket
on the adsorption column.
References
[1] Geankoplis, C. J., 2014. Transport Processes and Separation Process Principles. 4th
Ed ed. Delhi: PHI Learning.
[2] Seader, J. D., Henley, E. J. & Roper, D. K., 2010. Separation Process Principles. 3rd
Ed ed. Utah: Wiley.