CH3522: Unit Operations Laboratory, January-May 2025

ADSORPTION BREAKTHROUGH
GROUP 7
Madhumitha S(CH22B030), Vishal Dharsan V (CH22B027), Rohan S A (CH22B029),
Aayush Dhalwal (CH22B028)
Department of Chemical Engineering, Indian Institute of Technology Madras
ch22b030@[Link], ch22b027@[Link], ch22b029@[Link],
ch22b028@[Link]

Date of Experiment: 29/01/2025 Date of submission: 04/02/2025

1​ AIM

●​ Plotting of the breakthrough curve

●​ Estimation of the equilibrium capacity of the silica gel bed with water
●​ Estimation of the mass transfer coefficient using the breakthrough curve

2​ INTRODUCTION

​ Adsorption occurs when molecules from a gas of liquid stick to the surface of a
solid material, known as the adsorbent. In this experiment, we use silica gel as the
adsorbent and water vapour from humid air as the adsorbate. Adsorption happens
because of a difference in chemical potential between the fluid and the solid surface,
which causes the molecules to accumulate on the adsorbent. This process is driven by
weak forces between molecules, like van der Waals forces and hydrophobic interactions,
allowing it to be reversible. That means the silica gel can be reused after releasing the
adsorbed molecules, often through heating or drying.
​ However, the silica gel can only adsorb a limited amount of water vapour before it
becomes saturated. When this happens, the water vapour starts to pass through the
adsorbent and exits with the air. This point is called breakthrough. Understanding
breakthrough behaviour is essential for optimising silica gel columns in applications
like air dehumidification, gas purification and environmental cleanup.
​ By studying adsorption experimentally, we can learn more about how to design
and operate packed bed systems more efficiently. For industrial processes, it’s important
to know when breakthrough will occur to avoid system failures or inefficiencies.
Additionally, factors like temperature, humidity and air flow rate can affect the
adsorption process, and understanding these can lead to better system performance on a
larger scale.

3​ THEORY

​ Silica gel is a highly porous material with a large surface area, typically between
100 and 1200 m2/g, making it effective for adsorbing water vapour from humid air.
 CH3522: Unit Operations Laboratory, January-May 2025

Several factors influence its adsorption performance:

●​ Pore size and surface chemistry: these characteristics determine how well the
silica gel can trap water vapour
●​ Operating conditions: temperature and flow rate play a significant role.
Adsorption capacity decreases as temperature increases due to the exothermic
nature of the process.
●​ Particle size: smaller particles enhance mass transfer but may cause increased
pressure drop in the column.
●​ Humidity: higher inlet humidity leads to faster saturation of the silica gel.

​ Silica gel’s ability to adsorb water vapor is based on these properties, and it
eventually reaches a point where it becomes saturated and can no longer adsorb water
vapour effectively.

Mass Transfer Zone (MTZ)

​ In a packed bed adsorption column, the Mass Transfer Zone (MTZ)[1] is critical.
The MTZ is the region where active adsorption occurs. As humid air flows through the
silica gel bed, the MTZ moves along the column. The length of the MTZ is determined
by:
●​ Mass transfer rate: higher rates result in a shorter MTZ
●​ Fluid velocity: increased velocity can compress the MTZ
●​ Adsorbent properties: the structure and surface characteristics of the silica gel
also affect the MTZ behaviour.
​ A shorter MTZ signifies more efficient bed utilisation meaning the adsorbent’s
capacity is better utilised for adsorption.
 CH3522: Unit Operations Laboratory, January-May 2025

Figure 1: The Mass Transfer Zone (MTZ) indicated by black diagonal

Breakthrough Phenomenon

​ The breakthrough phenomenon occurs when the MTZ reaches the end of the
column, allowing the water vapour to escape with the effluent air. The breakthrough
curve, which plots the ratio of outlet to inlet concentration (C/C0) over time describes
this process: [2]
●​ Initial plateau: Adsorption is complete, and the effluent concentration is near
zero
●​ Breakthrough point: Adsorption sites near the column’s inlet become saturated,
allowing some water vapour to pass through
●​ S-shaped curve: this represents the progression of the MTZ as it moves through
the column
●​ Saturation plateau: the effluent concentration reaches the inlet concentration
(C/C0 = 1) indicating full saturation of the silica gel bed
 CH3522: Unit Operations Laboratory, January-May 2025

Figure 2: Breakthrough curve characteristics in the fixed bed column adsorption process over
time

Factors Affecting the Breakthrough Curve

​ Several factors influence the shape and timing of the breakthrough curve:
●​ Silica gel characteristics: surface area, pore size, and chemical composition
determine the adsorption capacity
●​ Operating conditions: temperature, flow rate and concentration of water vapour
affect when breakthrough occurs and how quickly the column saturates.
●​ Adsorbate properties: molecular size and popularity influence how quickly the
adsorbate reaches the saturation point.

Equilibrium Capacity of the Adsorption Bed

​ The equilibrium adsorption capacity of the silica gel in the packed bed is
calculated using the following equation:
𝑡𝑒
𝐶𝑜𝑢𝑡
𝑊𝑚𝑎𝑥 = 𝑄0 ∫(1 − 𝐶𝑖𝑛
(𝑡))𝑑𝑡 → (Equation 3)
0

Where:
●​ Wmax is the maximum adsorbed mass
●​ Q0 is the inlet flow rate
 CH3522: Unit Operations Laboratory, January-May 2025

●​ Cout and Cin are the outlet and inlet concentrations, respectively
●​ te is the time when saturation occurs
​ This formula helps determine the total amount of water vapour the silica gel can
adsorb before reaching saturation. Optimising the system based on this understanding
can improve efficiency in applications.

4​ APPARATUS REQUIRED

1. Activated Silica
2. RH Meter​
3. Glass Column​
4. Connecting Pipes​
5. Bubble Flow Meter
6. Balloon
7. Cotton Plug​
8. Retort Stand

5​ PROCEDURE AND SCHEMATIC DIAGRAM

Figure 3: The silica gel-packed column through which moist air is passed. An RH metre
is connected at the outlet to measure the outlet relative humidity.

​ Procedure:

1.​ Prepare a 5 cm glass column filled with activated silica, ensuring a cotton plug is placed
at both ends to prevent external airflow.
 CH3522: Unit Operations Laboratory, January-May 2025

2.​ Secure the column to a retort stand and connect one end to a bubble flow meter and the
other to a relative humidity (RH) meter using appropriate tubing.
3.​ Adjust the gas volumetric flow rate using a soap solution, balloon, and the assembled
setup.
4.​ Start the bubble flow meter and record the relative humidity readings at one-minute
intervals.
5.​ Capture a snapshot of the glass column every minute to track any color changes in the
silica over time.

6​ RESULTS AND OBSERVATIONS

Mass of silica gel=1.56 gm

Length of the packing = 5.5 cm
Diameter of the packing = 1.03 cm
Volumetric Flow rate of the gas= 0.743 ml/s
Inlet Relative Humidity = 64.5%

Table 1: Variation of relative humidity and mass of silica used up with time
Time Relative Ratio of white Ratio of white ms (mass of silica
(min) Humidity section packing section packing involved)
(%) (observed) (theoretical)

1 44.4 0.0005 0.00078

2 29.2 0.0012 0.0019

3 22.1 0.0109 0.017

4 18.4 0.0206 0.0321

5 15.9 0.0303 0.0473

6 14.0 0.04 0.0624

7 12.9 0.0497 0.0775

8 11.7 0.0594 0.0927

9 11.2 0.0691 0.1078

10 10.4 0.0788 0.1229

11 9.9 0.0885 0.1381

 CH3522: Unit Operations Laboratory, January-May 2025

12 9.5 0.0982 0.1532

13 9.2 0.1079 0.1683

14 9.0 0.1176 0.1835

15 8.5 0.127 0.1273 0.1986

16 8.5 0.137 0.2137

17 8.4 0.1467 0.2289

18 8.6 0.1564 0.244

19 8.3 0.1661 0.2591

20 8.3 0.1758 0.2742

21 8.2 0.1855 0.2893

22 8.1 0.1952 0.3044

23 7.9 0.2048 0.3196

24 8.0 0.2145 0.3347

25 7.9 0.2242 0.3498

26 7.8 0.2339 0.3649

27 7.8 0.2436 0.38

28 7.9 0.2533 0.3951

29 7.9 0.263 0.4103

30 7.9 0.273 0.2727 0.4254

31 8.0 0.2836 0.4424

32 8.0 0.2945 0.4595

33 8.0 0.3055 0.4765

34 8.0 0.3164 0.4936

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35 8.1 0.3273 0.5106

36 8.2 0.3382 0.5276

37 8.2 0.3491 0.5446

38 8.4 0.36 0.5616

39 8.4 0.3709 0.5786

40 8.6 0.3818 0.5956

41 8.6 0.3927 0.6126

42 8.7 0.4036 0.6297

43 8.7 0.4146 0.6467

44 8.9 0.4255 0.6637

45 8.9 0.436 0.4364 0.6808

46 9.0 0.44 0.6864

47 9.1 0.4436 0.692

48 9.3 0.4473 0.6978

49 9.3 0.4509 0.7034

50 9.5 0.4545 0.709

51 9.5 0.4581 0.7146

52 9.6 0.4618 0.7204

53 9.8 0.4654 0.726

54 9.9 0.4691 0.7318

55 10.1 0.4727 0.7374

56 10.3 0.4763 0.743

57 10.6 0.48 0.7488

 CH3522: Unit Operations Laboratory, January-May 2025

58 10.7 0.4836 0.7544

59 11.0 0.4873 0.7602

60 11.3 0.491 0.4909 0.7658

61 11.7 0.5036 0.7856

62 12.4 0.5163 0.8054

63 12.7 0.5291 0.8254

64 12.9 0.5418 0.8452

65 13.1 0.5545 0.865

66 13.3 0.5672 0.8848

67 13.6 0.58 0.9048

68 13.9 0.5927 0.9246

69 14.4 0.6055 0.9446

70 14.7 0.618 0.6182 0.9644

71 15.4 0.6309 0.9842

72 15.7 0.6437 1.0042

 CH3522: Unit Operations Laboratory, January-May 2025

Figure 4: Graph of relative humidity vs time

Since the relative humidity is the measure of the amount of water vapour present
in the outlet stream, we can approximate the Cout/Cin term with RH out/ RH initial term to get
the adsorption breakthrough curve.

Figure 5: Graph of Cout/Cin vs time

We have observed the fraction of white part, which symbolises the amount of
mass of silica gel that has been hydrated. We have observed those values for 15, 30, 45,
60, 70 minutes. So we have plotted the fraction of packed bed saturated vs time.
 CH3522: Unit Operations Laboratory, January-May 2025

Figure 6: Graph of fraction of silica used vs time

We can observe that after 60 minutes there is a steep increase in the amount of
water from humidity being adsorbed on silica, but before that the fraction of silica used is
gradual.
 CH3522: Unit Operations Laboratory, January-May 2025

Figure 7: Representation of fraction of white section packing at the time intervals of

t = 15, 30, 45, 60, 70 mins respectively

7​ SAMPLE CALCULATIONS

1. Estimation of Adsorption Coefficient

Assuming linear relationship between adsorbed water and concentration of water in air

𝑞𝑠𝑜𝑙𝑖𝑑 𝑚𝑤
𝐾𝑎ds = ρ𝑤
= 𝑚𝑠. ρ𝑤
→ (Equation 1)

Where mw mass of water adsorbed and ms is the mass of silica involved in adsorption. We
can assume all the moisture flowing inside is getting adsorbed initially, hence
ρ𝑤. 𝑄 . 𝑡 𝑄.𝑡
𝐾𝑎ds = ρ𝑤 . 𝑚𝑠
= 𝑚𝑠
→ (Equation 2)

𝑄, the mass flow rate of water = 𝑣𝑜𝑙𝑢𝑚𝑒𝑡𝑟𝑖𝑐 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒 × 𝐶𝑖𝑛 = 0.743 × 10-6 g/s.

The inlet concentration was obtained using the Magnus relation from relative humidity
and wet bulb temperature data.

For example,. 𝑚𝑠 at t = 6 mins, is 1.56 × 0.04 = 0.0625 g

Substituting the values we obtain
 CH3522: Unit Operations Laboratory, January-May 2025

𝐾𝑎ds = 7.13 × 10-5

2. Estimation of Maximum Adsorption Capacity

Using the trapezoidal rule, in order to evaluate the definite integral

𝑡𝑒
𝑐𝑜𝑢𝑡
𝑊𝑚𝑎𝑥 = Q ∫(1 - 𝑐𝑖𝑛
(t)) dt → (Equation 3)
0
We obtain maximum adsorption capacity to be 7.088 × 10−5 𝑔.

8​ CONCLUSION AND DISCUSSION

●​ As time progresses, the sensor detects outlet air from the packed bed, forming the
breakthrough curve.
●​ At the start, the unsaturated silica gel fully adsorbs the water vapour, keeping the outlet
humidity near zero.
●​ The breakthrough point marks the saturation of the mass transfer zone, allowing some
water vapour to escape.
●​ Once the silica gel is fully saturated, the curve flattens indicating no further adsorption.
●​ The gradual rise after the breakthrough point suggests non-ideal flow, likely due to
internal resistance in the packed bed.
●​ Since adsorption depends on airflow rate, increasing it would enhance the process and
increase the total amount adsorbed.

9​ REFERENCES

[1] Gabelman, A., Gabelman Process Solutions, LLC, & American Institute of Chemical
Engineers (AIChE). (2017). Adsorption Basics: Part 1. CEP, 49.
[Link]
[2] Prompted with “Breakthrough curve for silica gel packed bed”
​​ OpenAI. (2025). ChatGPT.
​​ [Link]
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CH3522: Unit Operations Laboratory, January-May 2025