1.

0 ABSTRACT

The objective of the experiment was to study the adsorption in a packed bed for a solid liquid
system. This is done by plotting the breakthrough curve of adsorption for a given system and
then calculating the length of unused bed for the given system. The set-up consists of three
borosilicate columns having different diameters & lengths. For flow of fluid a pump & rotameter
is provided. At the inlet of column, valves are provided to feed only one column at a time. Valves
are provided at the bottom of columns & liquid tanks to drain out after running the apparatus.
Filters are provided before the column drain valves to prevent the charcoal from drain. In order
to achieve the aims and objective of the experiment a packed bed of length 1.0m filled with
activated charcoal was used. A colored liquid of Potassium permanganate (KMnO4) was passed
through the bed under a constant flow rate of 10LPH and temperature. Samples of the colored
liquid were collected at 10 minute intervals till the liquid color was consistent. The color of the
liquid became fairly consistent after 60 minutes and 10 minutes later, no change was noticed.
The samples absorbance was measured used a UV spectrophotometer which detected the
capacity of the liquid to absorb light. The initial adsorbance detected was 3 while the final was
0.292. The wavelength of the uv-light passed through the samples was also constant at 526 cm.
The initial concentration of potassium permanganate (KMnO4) was calculated to be 0.9308
which is also the concentration of the feed. While the final concentration reading was 0.0906.
The Breakpoint time (B) was found to be 10 minutes while the Ideal time ( S) was 30 minutes,
giving the length of unused bed was found to be 0.6667m.
2.0 INTRODUCTION

2.1 Theory

Adsorption is the selective transfer of an adsorbent solute from a fluid phase to a batch of rigid
particles. The usual selectivity of an adsorbent between solute and carrier fluid or between
different solutes makes it possible to separate certain solutes from the carrier or from one
another.
It occurs when molecules diffusing in the fluid phase are held for a period of time by forces
emanating from an adjacent surface. The surface represents a gross discontinuity in the structure
of the solid, and atoms at the surface have a residue of molecular forces which are not satisfied
by surrounding atoms like those in the body of the structure.
These residual or Vander Waals forces are common to all surface and the only reason that certain
solids are designated "adsorbents" is that they can be manufactured in a highly porous form,
giving rise to a large internal surface. Few fixed beds have internal probes that would permit
measurement of profiles such as concentration profile. However these profiles can be predicted
and used in calculating the curve of concentration versus time for fluid leaving the bed. The type
of curve is called break through curve.
Length of unused bed can be calculated as:

L(S B)
LUB=
S

Where L, S ,B and LUB are total length of bed, ideal time, break point time and length of unused
bed. B can be calculated from the above graph, it is the time where some minimum
concentration shows. S can also calculated from the above graph, it is determined in a way that
the areas of the shaded portions are equal.

2.2 Advantages, Disadvantages and Applications of Adsorption in Packed bed.

Adsorption in packed bed is advantageous in many ways. Firstly, adsorption in packed bed is
relatively cheap in such a way that the activated charcoal used in the first stream can be reused
again. This reduces the expenditure on buying activated charcoal for the experiment. This packed
(fixed) bed equipment is a simple equipment which makes it easy to use. It is also easy to collect
the samples from the bed due to the simplicity of the equipment construction which saves time.
The upstream flow of the liquid into the bed provides a considerably large surface area for
adsorption to take place.
However, the adsorption in packed bed has disadvantages too. The adsorption is ineffective if the
flow of the liquid is downstream. This is because the amount of time the liquid spends inside the
bed small. In a solid-liquid system, the adsorption of the liquid depends on a lot of factors such
as, temperature, pressure, nature of absorbent, surface area of adsorbent and the nature of
adsorbate. Therefore, any slight variation in the following can affect the whole entire process
which in turn affects the results.
Adsorption in packed bed is used for various purposes such as, in heterogeneous catalytic
process, gas masks where activated charcoal adsorbs poisonous gases, the refining of petroleum
and decolouring cane juice. It is also employed in creating vacuum by adsorbing gases on
activated charcoal, in chromatography to separate the constituents of a mixture, to control
humidity by the adsorption of moisture on silica gel and certain titrations to determinate the end
point using an adsorbent as indicator (Example: Flouroscein).
3.0 PROCEDURE

3.1 20 liter of colored liquid was prepared by dissolving known amount of KMnO4 in 20 liter of
water.

3.2 Valves V1-V10 are all closed.

3.3 The switches given on the panel were ensured that they were at the OFF position.

3.4 The feed tank was filled with the colored liquid.

3.5 Activated charcoal was kept in all columns.

3.6 The electric supply was connected to the set-up.

3.7 The valve V3 of the column-1 was opened.

3.8 The bypass valve V2 was partially opened.

3.9 The pump was switched ON.

3.10 The flow control valve V1 and bypass valve V2 were opened and adjusted.

3.11 The stop watch was started simultaneously.

3.12 Samples were collected from outlet of column 1 after a time interval.

3.13 The time was noted down.

3.14 The optical densities of the samples were measured.

3.15 The experiment was let to run till the change in color of outlet liquid becomes almost stable.

3.16 The valve V3 was closed.

3.17 The valve V4 of the column-2 was now opened.

3.18 The stop watch was started simultaneously.

3.19 The samples were collected from the outlet of column-2 after a time interval.
3.20 The time was noted down.

3.21 The adsorbance of these samples were measured.

3.22 The experiment was let to run till the change in color of outlet liquid becomes almost stable.

3.23 The valve V4 was closed.

3.24 The valve V5 of the column-3 was opened.

3.25 The stop watch started simultaneously.

3.26 The samples were collected from the outlet of column-3 after a time interval.

3.27 The time was noted down.

3.28 The adsorbance of these samples were measured.

3.29 The experiment was let to run till the change in color of outlet liquid becomes almost stable.

3.30 The valve V5 was closed.

3.31 When the experiment was over the supply of feed was stopped by closing the valve V1.

3.32 The pump was switched OFF.

3.33 The main power supply was switched OFF.

3.34 The columns were drained by opening the valve V6, V7 and V8.

3.35 The feed tank was drained by opening the valve V9.

3.36 The product tank was drained by opening the valve V10.

3.37 The charcoal was removed by opening the filter cups of the column properly.

Calculations were done using the following formulae;

 Figure 3.1: Apparatus used in adsorption of packed bed.

Figure 3.2: Block diagram of apparatus.

4.0 RESULTS AND DISCUSSION

Table 4.1: Standard Concentration and Absorbance

Concentration (ppm) ABS

0 0
0.01 0.019
0.02 0.075
0.03 0.093
0.04 0.135
0.05 0.161
0.06 0.190

Table 4.2: Observation table for showing adsorbance at 10 minute intervals.

(min) ABS
 0 3.000
10 2.962
20 3.000
30 3.000
40 2.296
50 0.399
60 1.850
70 0.292

Table 4.3: Experimental adsorbance value and Concentration with time.

(min) CS C=CF-CS C/CF

0 0.9308 (CF) 0.0000 0.0000
10 0.9190 0.0118 0.0127
20 0.9308 0.0000 0.0000
30 0.9308 0.0000 0.0000
40 0.7124 0.2184 0.2346
50 0.1238 0.8070 0.8670
60 0.5740 0.3568 0.3833
70 0.0906 0.8402 0.9027

The experiment was conducted in order to study the adsorption in a packed bed for a solid liquid
system which is the main objective of the experiment. This is done by plotting the breakthrough
curve of adsorption for a given system and also by calculating the length of unused bed for the
given system. In this case activated charcoal was used as the adsorbent and the potassium
permanganate (KMnO4) of unknown concentration was the colored liquid that was used as the
adsorbate. The length of the column that was used in this experiment is 1.0 m and filled with the
activated charcoal pellets. The activated charcoal pellets was used as the packed bed through
which potassium permanganate was allowed to flow through it at a constant flow rate of 10 LPH.

Adsorption is a process where the adhesion of atoms or molecules of gas, liquid or dissolved
solid (adsorbate) on a surface (adsorbent). Absorption on the other hand is when the substance
such as a liquid or a solid (absorbent) takes up another substance such as a liquid or a gas
(absorbate) through spaces or pores of its molecules. When speaking of the difference between
these two processes, is that in adsorption, no new chemical structure is formed whilst in
absorption a new chemical structure is formed. Therefore, in order to investigate adsorbance of
the colored liquid, a table of standard values and absorbance to a plot of graph of best fit which
shows the relationship between concentration and absorbance (ABS). The values that were used
to plot the graph shown below are shown in table 3.1.

0.2
0.18 f(x) = 3.22x

0.16
0.14
0.12

ABS 0.1
0.08
0.06
0.04
0.02
0
0 0.01 0.02 0.03 0.04 0.05 0.06 0.07

Concentration

Figure 4.1: Graph of absorbance with respect to concentration using standard values given.

Absorbance is the capacity of a substance to absorb light. Therefore, the relationship between
absorbance and concentration is that, the high the absorbance, the more concentration the
solution. Samples of the colored liquid were collected every 10 minutes till the color was almost
constant. This was to investigate the amount of dissolved solution which was adsorbed by the
activated charcoal. The more the liquid was adsorbed, the more concentrated the remaining
solution was. This is due to the fact that, the liquid adsorbed by activated charcoal contained a
huge amount of water and less of potassium permanganate compared to the one collected from
the column. Hence, the longer the time taken to collect the liquid, the more concentrated it
became till the activated charcoal became saturated and could no longer adsorb the liquid. The
results below show the change the liquid concentration and absorbance with time.

With the equation obtained from the graph above, the concentration of samples that were
collected at 10 minute intervals were calculated as shown in the appendix. The experimental
values obtained are as shown in table 3.3. These values were then used to plot a graph which
helps in better understanding of how the concentration of colored liquid differed with time.

1
0.9
0.8
0.7
0.6

C/CF 0.5
0.4
0.3
0.2
0.1
0
0 10 20 30 40 50 60 70 80

Time (min)

Figure 4.2: The breakthrough curve showing the relationship between concentration of
liquid and time.

It was observed that the though the values fluctuated, generally the concentration of the colored
liquid decreased with time. The graph was plotted using the ratio of difference of concentration
feed (CF) and the concentration of samples (C S) with time. The fluctuations in the values of
concentration may have been due to the unstable flow rate of the feed. The fluctuations might
have also been caused by errors made when placing the liquid samples in the spectrophotometer
used to measure the absorbance of the liquid. As it is known that the absorbance of a liquid is a
function of its concentration. Ultimately, the concentration of Potassium permanganate increased
with time. This was also noticed by the change of color of the liquid as time passed; thereby
confirming that adsorption was taking place. However, at the 60th minute of collecting the
samples, it was noticed that there was a dip in the curve showing that and error might have
occurred when conducting the experiment. Which may be caused by lack of feed sample in the
apparatus or even increasing the flow rate of the colored liquid. Thus, by doing this, it disrupts
the flow and dynamics of the apparatus to produce ideal results.
But in an ideal situation, the curve from the 60 th to the 70th minute was meant to be almost
forming a straight line proving that the colored liquid was stabilizing, which could be deduced by
observing the almost constant color change between these two respective time intervals. This
behavior also meant that the activated charcoal in the packed bed was saturated and could no
longer adsorb the liquid.
The Breakpoint time (B) was 10 minutes and the Ideal time ( S) was 30 minutes when the
system was now stable giving the length of the unused bed (LB) to be 0.6667m.

5.0 CONCLUSION AND RECOMMENDATION

The experiment, adsorption in packed bed was conducted to study the adsorption in a packed for
a solid-liquid system. The aims of the experiment were to plot the Breakthrough curve of
adsorption for a given system and to calculate the length of the unused bed for a given system. In
this experiment, activated charcoal was used as the adsorbent and a liquid of potassium
permanganate (KMnO4) in water was the adsorbate. Eight different samples of the liquid were
collected every 10 minutes and the absorbance of the liquid sample was measured using UV
spectrophotometer. The experiment was conducted under constant temperature and pressure. The
Breakthrough curve was plotted which gave the Breakpoint time ( B) as 10 minutes and the Ideal
time (S) as 30 minutes. The length of the unused bed was calculated to be 0.6667m. The
objective and aims of this experiment were achieved and therefore, the experiment was a success
within the margin of problem encountered and errors made.
However, there were some errors made during the experiment. The initial sample of the colored
liquid was not collected at the right time. This affected the values of concentration calculated
every 10 minutes. The fluctuations in the values of absorbance recorded showed that the samples
were not taken at exact time interval and that the flow rate of the feed was fluctuating. The
values of absorbance recorded could have fluctuated due to the wrong positioning of the sample
holders when placing them in the UV spectrophotometer. Collecting samples of constant volume
at a small amount also helps in maintaining the amount of feed that is contained in the apparatus
and hence also maintaining the flow rate.
Therefore, to avoid such errors being made both at experimental and industrial level, great care
should be taken when performing the adsorption in packed bed. It should be ensured that the
initial sample of the adsorbate is collected before being put in the column containing the
adsorbent. It should also be ensured that the flow rate of the adsorbate is monitored and kept
constant throughout the experiment. Ensure that all external factors such as temperature and
pressure are also monitored for any slight change in these factors may affect the adsorption
especially in gas-solid and gas-liquid systems. When placing the liquid sample holders in the UV
spectrophotometer, it should be ensured that the smooth surface of the holder face the open side
so that the UV light can pass through the liquid.

6.0 REFERENCES

1 Warren L. McCabe, Julian C. Smith and Peter Harriott, Unit Operations of Chemical
Engineering, McGraw-Hill, 2005.

2 Coulson, J.M. and Richardson, J.F., Chemical Engineering, Vol. II (Particle Technology
and Separation Processes), Pergamon, 1991.

3 Geankoplis, C.J., Transport Processes and Unit Operations, 3 rd ed., Prentice-Hall

International Inc., 1978.
4 Foust, A.S., Wenzel, L.A., Clump, C.W., Maus, L. and Anderson, L.B., Principles of
Unit Operations, 2nd ed., John Wiley, New York, 1980.

5 Sinnott, R. K., Chemical Engineering Design: Principles,, Practice and Economics of

Plant and Process Design, 2nd ed., Butterworth-Heinemann, 2012, p. 807

7.0 APPENDIX

The length of column used was 1.0 m. The calculations shown below are at the 60th minute.

Equation of the line:

y = 3.2231x
At 70 minutes,
CF = 0.9308
Cs = 3.2231(1.850) = 0.5740
C = 0.9308 0.5740
= 0.3568
C/CF = 0.3568/0.9308
= 0.3833