ENGI 9628 Environmental Laboratory

Lab 6: Adsorption

Objective
To evaluate the effectiveness of adsorption in removing dyes such as Methylene Blue.

Theory
Dyes, such as Methylene Blue, Crystal Violet, Congo Red, and Rhodamine, are widely used in various
industries, including textile, printing, and pharmaceuticals. However, the discharge of these dyes into the
environment poses a significant threat due to their toxic and persistent nature. Traditional wastewater
treatment methods are often ineffective in removing these dyes completely, leading to the contamination
of water bodies and adverse effects on aquatic life and human health. Therefore, the development of
efficient and eco-friendly techniques for dye removal is important. Adsorption has emerged as a promising
approach for the removal of dyes from wastewater. It is a widely studied phenomenon in which
contaminants are physically or chemically attracted to a solid surface, resulting in their attachment and
removal from the solution. The adsorption process is governed by various factors such as the surface
properties of the adsorbent, dye concentration, pH, temperature, and contact time. The choice of
adsorbent material is crucial as it determines the effectiveness of the dye removal process.
Adsorbents used for dye removal can be broadly categorized into two types: natural and synthetic. Natural
adsorbents include materials such as activated charcoal, chitosan, zeolites, and certain clays. These
materials offer advantages such as abundance, low cost, biodegradability, and potential renewability.
Synthetic adsorbents, on the other hand, are typically engineered materials with modified surface
properties and specific functional groups to enhance their adsorption capacity and selectivity.
Investigating the adsorption potential of different adsorbents for dye removal not only provides insights
into the fundamental aspects of the adsorption process but also contributes to the development of
sustainable and cost-effective methods for wastewater treatment, ensuring the protection of the
environment and human health.

Reagents
1. Distilled or deionized water
2. Water sample containing dye contaminants (Methylene Blue: 50 mg/L)
3. Adsorbent (biochar derived from coconut shells)
4. Distilled water
5. Hydrochloric acid (HCl) and sodium hydroxide (NaOH) solutions (1 M, 0.1 M)

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 ENGI 9628 Environmental Laboratory
Lab 6: Adsorption

Apparatus
1. Jar test
2. Beaker, 600 mL
3. Spectrophotometer
4. Test tubes or cuvettes
5. Measuring columns (100 ml)
6. Disposable pipette
7. Stopwatch
8. pH meter
9. Balance
10. Paper filter

Procedure
1. Preparation of Standards: Prepare a series of standard solutions with known concentrations of
the dye using distilled water. Use a stock solution of the dye and dilute it to obtain standard
solutions with different concentrations. Prepare at least four standards with known
concentrations covering the expected range of dye concentrations. (provided by TA)
2. Jar Test Procedure: The jar test is a common laboratory procedure used to determine the
optimum operating conditions for water or wastewater treatment. This method allows
adjustments in pH, variations in adsorbent dose, mixing speeds, time, initial concentration of the
contaminant, etc.
The jar test procedures involve the following steps:
• Fill the jar testing apparatus containers with sample water (300 ml) using measuring cylinders.
• Add the required amount of adsorbent to each container and stir at approximately 130 rpm for
1h.
• Turn off the mixers.

Figure 1. Diagram of jar testing device

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Lab 6: Adsorption

Each group will conduct one specific experiment from the following options:

Experiment 1: Effect of the Dye Initial Concentration

• Prepare six beakers with 300 mL of distilled water each in the jar tester.
• Add 0.3 g/L of the adsorbent to each beaker.
• Add varying initial concentrations of methylene blue (10, 15, 20, 25, 30, 35 mg/L) to each
beaker.
• Stir the solutions using the jar tester for one hour.
• After one hour, stop the stirring and allow the particles to settle.
• Filter the solutions using filter paper.
• Measure and record the absorbance of the filtrate using a UV spectrophotometer at 660 nm.

Experiment 2: Effect of Adsorbent Dose

• Prepare six beakers with 300 mL of distilled water each in the jar tester.
• Add a constant concentration of methylene blue (25 mg/L) to each beaker.
• Add varying doses of the adsorbent (0.1, 0.2, 0.3, 0.4, 0.5, 0.6 g/L) to each beaker.
• Stir the solutions using the jar tester for one hour.
• After one hour, stop the stirring and allow the particles to settle.
• Filter the solutions using filter paper.
• Measure and record the absorbance of the filtrate using a UV spectrophotometer at 660 nm.

Experiment 3: Effect of pH
• Prepare six beakers with 300 mL of distilled water each in the jar tester.
• Add a constant concentration of methylene blue (25 mg/L) and 0.3 g/L of the adsorbent to
each beaker.
• Adjust the pH of each solution to 2, 4, 6, 8, 10, 12 using HCl and NaOH solutions (1 M, 0.1 M).
• Stir the solutions using the jar tester for one hour.
• After one hour, stop the stirring and allow the particles to settle.
• Filter the solutions using filter paper.
• Measure and record the absorbance of the filtrate using a UV spectrophotometer at 660 nm.

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Lab 6: Adsorption

Experiment 4: Effect of Time

• Prepare six beakers with 300 mL of distilled water each in the jar tester.
• Add a constant concentration of methylene blue (25 mg/L) and 0.3 g/L of the adsorbent to
each beaker.
• Stir the solutions using the jar tester for varying durations (10, 20, 30, 40, 50, 60 minutes).
• After each designated time, stop the stirring and allow the particles to settle.
• Filter the solutions using filter paper.
• Measure and record the absorbance of the filtrate using a UV spectrophotometer at 660 nm.
Experiment 5: Effect of mixing speed
• Prepare six beakers with 300 mL of distilled water each in the jar tester.
• Add a constant concentration of methylene blue (25 mg/L) to each beaker.
• Add varying doses of the adsorbent 0.3 g to each beaker.
• Set the mixing speed to 50, 75, 100, 125, 150, and 175 rpm.
• Stir the solutions using the jar tester for 15 minutes for each mixing speed.
• After one hour, stop the stirring and allow the particles to settle.
• Filter the solutions using filter paper.
• Measure and record the absorbance of the filtrate using a UV spectrophotometer at 660 nm.

Calculation
1. Prepare a calibration curve by plotting instrument response against standard concentration of the
dye.
Standard # Concentration (mg/L) Absorbance
1 0.1 0.016
2 0.2 0.021
3 0.4 0.036
4 0.6 0.074
5 0.8 0.085
6 1 0.161

2. Compute sample concentration by comparing sample response with the standard curve.

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Lab 6: Adsorption
3. Calculate the percentage removal of the dye using Equation (1).
Removal (%) = [(Ci - Cf) / Ci] × 100 (1)
Where
Ci = the initial dye concentration in the water sample.
Cf = the final dye concentration after adsorption.

4. Create a figure that visually represents the effects of the experimental parameter (x-axis) on
adsorption efficiency (y-axis). Specifically, design a graph for each experiment (initial
concentration, adsorbent dose, pH, contact time, and mixing speed). Additionally, mark the point
on each graph that represents the optimum condition where adsorption efficiency is maximized.
5. After analyzing the effects of various parameters on adsorption efficiency, it is essential to explore
the practical applications and implications of these findings. Consider adding a section that
discusses the potential real-world applications of the adsorption process optimized through your
experiments.
6. Compare your results with some results from published literature.
7. Discuss your results.

Learn more by exploring the following key references:

1- Akash, M. S. H., Rehman, K., Akash, M. S. H., & Rehman, K. (2020). Ultraviolet-visible (UV-VIS)
spectroscopy. Essentials of pharmaceutical analysis, 29-56.
2- Dutta, S., Gupta, B., Srivastava, S. K., & Gupta, A. K. (2021). Recent advances on the removal of
dyes from wastewater using various adsorbents: A critical review. Materials Advances, 2(14),
4497-4531.
3- Kadhom, M., Albayati, N., Alalwan, H., & Al-Furaiji, M. (2020). Removal of dyes by agricultural
waste. Sustainable Chemistry and Pharmacy, 16, 100259.
4- Sultana, M., Rownok, M. H., Sabrin, M., Rahaman, M. H., & Alam, S. N. (2022). A review on
experimental chemically modified activated carbon to enhance dye and heavy metals
adsorption. Cleaner engineering and technology, 6, 100382.