B49CE Multiphase Thermodynamics

B49CD Separation Process B

Heriot-Watt University
School of Engineering and Physical Science
Chemical Engineering

Stage 3 Laboratory Experiment

Experiment 8(OEL): Absorptive Removal of Basic Dye from
Aqueous Solution Using Fruit Waste as Biosorbent

Group 5
Name Student ID
Lee Ci Wei H00255305
Haziq Khairin Adham bin Hasni H00261346
Leonard Lim Tuck Wah H00283746

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 Heriot-Watt University
School of Engineering and Physical Science
Chemical & Petroleum Engineering

B49CE Multiphase Thermodynamics

B49CD Separation Process B

Open-Ended Lab II
Absorptive Removal of Basic Dye from Aqueous Solution Using Fruit Waste as
Biosorbent

Contents

1 Introduction……………………………………………………………………………………... 2
2 Objectives………………………………………………………………………………………. 4
3 Apparatus and materials………………………………………………………………………. 4
4 Methodology……………………………………………………………………………………. 5
5 Experimental data sheet………………………………………………………………………. 7
6 Safety Note……………………………………………………………………………………… 10
7 Reference……………………………………………………………………………………….. 11

1 Introduction

Water pollution is a major problem facing the world today as water filtration systems are not
designed to filter out particles as small as methylene blue. Acute exposure to Methylene
Blue can cause a number of health problems. These include increase in heart rate, vomiting,
diarrhoea, nausea and shock (Drugs, 2018). An emerging market to solve this problem is
biomass adsorption using materials such as fruit skin, which adsorb the contaminant such as
dye in the process of purifying water.

In this experiment, the main objective is to determine the amount of methylene blue (MB)
adsorbed and percentage removal of methylene blue at different pH over a specific time with
the amount of biosorbent kept constant. Biosorbent, in which lemon skin will be used, have
to be prepared before carrying out the experiment. Lemon skin is grind into powder form and
used as biosorbent to remove methylene blue in the solution. Methylene blue is set at
different pH and determine the optimum pH of the methylene blue that is removed by
prepared biosorbents. The findings will then be recorded, tabulated and then graphed.

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In theory, the concentration of the Methylene Blue can be determined through the use of
Beer-Lambert law, in which UV-Vis spectrophotometer is used to determine values of the
absorbance of light. In determining the light intensity of both reference and sample cell, the
value of the concentration of methylene blue can be found through graphing and series of
equations. Once the initial and subsequent concentration have been determined, the
percentage of Methylene Blue removed can be calculated.

To calculate the following variables, the following equations will be used

(chemguide, 2007)

where I0 is the light intensity passing through reference cell and I is the experimental light
intensity passing though sample cell.

Beer-Lambert’s law: 𝐴 = 𝜀𝐼𝑐 (chemguide, 2007)

Where A is the absorbance of light, 𝜀 is the molar absorptivity (L/mol cm), l is the length
of solution the light passes through (cm) and c is the concentration of the solution (mol/dm3).

Percentage of methylene blue removed:

%R = ((co-ce)/co) ✕100% (Shakoor, 2016)

Where %R is the percentage of methylene blue removed (%), co is the initial concentration of
the methylene blue solution (mol/L), ce is the equilibrium concentration of the methylene blue
solution (mol/L).

In determining the amount of Methylene Blue being adsorbed (qe), the following equation will
be used

(Shakoor, 2016)

in which C0 and Ce is the concentration of MB initially and at equilibrium respectively in

mg/L and m is mass of adsorbent in grams and V is the volume of solution in Litre. Once
calculated, the amount of methylene can be found.

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2 Objectives

To determine the amount of methylene blue (MB) adsorbed and percentage removal of
methylene blue at different pH over a specific time while the amount of biosorbent used is
kept constant.

3 Apparatus and Materials

Apparatus

a. pH meter
b. UV-Vis Spectrophotometer
c. Blender
d. Oven
e. Electronic mass balance
f. Incubators shakers
g. Stopwatch
h. Magnetic stirrer plates
i. Retort stand and clamp
j. Conical flask (2 units)
k. Burette
l. 50 mL beaker (2 units)
m. 250 mL beaker (6 units)
n. 500 mL beaker (2 units)
o. 1L beaker (1 units)
p. Conical flask to be placed in the incubator shaker (5 units)
q. 250 mL measuring cylinder (1 unit)
r. 1 L measuring cylinder (1 unit)
s. Spatula
t. Dropper
u. Sealed plastic bag / container

Materials

a. Sodium hydroxide, NaOH

b. Hydrogen chloride, HCl
c. Methylene Blue, C16H18ClN3S
d. 5 lemons
e. Universal Indicator

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4 Methodology

(a) Preparing biosorbent powder

1. Prepare 5 lemons and peel of the skin.

2. Wash the lemon skin with distilled water many times to remove the dust impurity.
3. Cut the lemon skin into small pieces around 2-3 cm.
4. Dry lemon skins using an oven for 24 hours at 100°C.
5. After 24 hours, take the lemon skins out from the oven and let them cool down for
about 5 minutes.
6. Grind the lemon skins using a blender until it become fine powder.
7. Keep the grinded lemon skins in a sealed plastic bag.

(b) Preparing the calibration curve to find the absorbance of the Methylene Blue

1. Prepare different concentrations of methylene blue at 0 mol/L, 0.2 mol/L, 0.4 mol/L,
0.6 mol/L, 0.8 mol/L and 1.0 mol/L.
2. Use the UV-Vis spectrophotometer to measure the absorbance of light of the
methylene blue solution.
3. Plot a graph of absorbance against concentration of methylene blue to obtain the
calibration curve.

Molar Mass of Methylene Blue =319.85 g/mol

Solution Mixture
Concentration of Absorbance
Methylene Blue (mol/L) Mass of MB solid Volume of H2O (ppm)
(g) (L)

0.0 0.00 0.05

0.2 1.59 0.05

0.4 6.40 0.05

0.6 9.60 0.05

0.8 12.80 0.05

1.0 16.00 0.05

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(c) Preparing the acidic and basic Methylene Blue (MB)

Note: when preparing acids and bases, PPE attire, inclusive of gloves and facial masks, is
REQUIRED to prevent injuries/accidents from occurring.

1. Record the absorbance of light of the methylene blue solution using the UV-Vis
Spectrophotometer.
2. Fill in 100 mL of 0.2 mol/L methylene blue solution in each 5 250 ml beakers and
label them as A, B, C, D and E.
3. Prepare 150 mL of 1 mol/L of HCl and 150 mL of 1 mol/L of NaOH and pour them
into their respective 250 mL beakers.
4. Mix methylene blue with NaOH and HCl to get corresponding pH values and
measure the pH of the methylene blue solution using a pH meter.
5. Add the acid or base into all five beakers (A-E) so that the pH of each beaker will
have the following pH values:

Beaker Corresponding pH values Remarks

A 3 Strong acid

B 5 Weak acid

C 7 Neutral

D 9 Weak base

E 11 Strong base

6. For Beaker C, methylene blue is poured into a conical flask with 5 drops of universal
indicator and titration is carry out to neutralise the solution.

(d) Removing methylene blue in aqueous solution using prepared biosorbents.

1. Add the same mass of biosorbent powder into all 5 of the beakers and stir using the
magnetic stirrer plates for 3 minutes.
2. Pour 70 mL of different pH methylene blue solution into separate conical flask and
place in an incubator shaker.
3. Use the UV-Vis spectrophotometer to record the absorbance value every 5 minutes
for 30 minutes, then leave the conical flask in incubator shaker for 72 hours and
record the absorbance value for every 24 hours intervals
4. Calculate the concentration of the methylene blue solutions using Beer-Lambert's
Law.
5. After calculating the concentrations of the methylene blue solutions, calculate the
percentage removal of methylene blue and amount of methylene blue adsorbed.

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 5 Experimental Data Sheet

Initial concentration of Methylene Blue: g/L

Initial intensity of Methylene Blue:
Initial absorbance of Methylene Blue: ppm
Length of solution that light passes through: cm3

pH 3
Time after lemon
Final
has been mixed Intensity of Volume of Amount of % of removal of
Absorbance concentration
with Methylene the Methylene Blue Methylene Blue Methylene Blue,
(ppm) of solution
Blue(min) adsorption (ml) adsorbed, q %R
(mol/dm3) e

5
10
15
20
25
30
1440(24 hrs)
2880 (48 hrs)
4320 (72 hrs)

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 pH 5
Time after lemon
Final
has been mixed Intensity of Volume of Amount of
Absorbance concentration % of removal of
with Methylene the Methylene Blue Methylene Blue
(ppm) of solution Methylene Blue
Blue(min) adsorption (ml) adsorbed, q
(mol/dm3) e

5
10
15
20
25
30
1440(24 hrs)
2880 (48 hrs)
4320 (72 hrs)

pH 7
Time after lemon
Final
has been mixed Intensity of Volume of Amount of
Absorbance concentration % of removal of
with Methylene the Methylene Blue Methylene Blue
(ppm) of solution Methylene Blue
Blue(min) adsorption (ml) adsorbed, q
(mol/dm3) e

5
10
15
20
25
30
1440(24 hrs)
2880 (48 hrs)
4320 (72 hrs)

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 pH 10
Time after lemon
Final
has been mixed Intensity of Volume of Amount of
Absorbance concentration % of removal of
with Methylene the Methylene Blue Methylene Blue
(ppm) of solution Methylene Blue
Blue(min) adsorption (ml) adsorbed, q
(mol/dm3) e

5
10
15
20
25
30
1440(24 hrs)
2880 (48 hrs)
4320 (72 hrs)

pH 13
Time after lemon
Final
has been mixed Intensity of Volume of Amount of
Absorbance concentration % of removal of
with Methylene the Methylene Blue Methylene Blue
(ppm) of solution Methylene Blue
Blue(min) adsorption (ml) adsorbed, q
(mol/dm3) e

5
10
15
20
25
30
1440(24 hrs)
2880 (48 hrs)
4320 (72 hrs)

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6 Safety Precautions
1) Personal protective equipment (PPE) must always be worn throughout the experiment.
2) Inspect all the equipment and make sure it is in good condition before using it.
3) Handle electrical equipment with care and do not touch it with wet hands.
4) Follow procedures of the operating manual for each equipment.
5) The pH meter’s electrode is fragile and should not be used as a stirrer.
6) Prepare concentrated alkaline and acid in the fume chamber.
7) Chemical waste have to be disposed off properly in the provided container.
8) Any incidents should be reported to the lab instructors.

Methylene Blue Sodium Hydroxide Hydrochloric Acid

FIGURE 1: National Fire Protection Association (NFPA) code for chemicals used

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7 Reference

Chemguide. 2016. absorption spectra- the Beer-Lambert Law. [ONLINE] Available at:
https://www.chemguide.co.uk/analysis/uvvisible/beerlambert.html. [Accessed 17 January
2019].

Lazim, Z.M., Mazuin, E., Hadibarata, T., Yusop, Z, 2015. The Removal of Methylene
Blue and Remazol Brilliant Blue R Dyes By Using Orange Peel and Spent Tea Leaves.
Jurnal Teknologi (Science and Engineering), [Online]. 74/11, p.p. 129-135. Available at:
https://www.researchgate.net/publication/279861618_THE_REMOVAL_OF_METHYLEN
E_BLUE_AND_REMAZOL_BRILLIANT_BLUE_R_DYES_BY_USING_ORANGE_PEEL
_AND_SPENT_TEA_LEAVES[Accessed 18 January 2019].

Kucic, D., Miljanic, S., Rozic, M., 2011. Sorption of Methylene Blue Onto Orange And
Lemon Peel. The Holistic Approach to Environment, 1/2, p.p. 41-51.

Malik, D.S., Jain, C. K., Yadav, A. K., Kothari, R., Pathak, V. V., 2016. Removal of
Methylene Blue Dye in Aqueous Solution by Agricultural Waste. International Research
Journal of Engineering and Technology, [Online]. 3/7, p.p. 864-880. Available at:
https://www.researchgate.net/publication/309040775_Removal_of_methylene_blue_dye
_in_aqueous_solution_by_agricultural_waste[Accessed 18 January 2019].

Shakoor, S., Nasar, A., 2016. Removal of methylene blue dye from artificially
contaminated water using citrus limetta peel waste as a very low cost adsorbent. Journal
of the Taiwan Institute of Chemical Engineers, [Online]. 66/1, p.p. 154-163. Available at:
https://www.sciencedirect.com/science/article/pii/S1876107016301742 [Accessed 15
January 2019].

Drugs. 2019. Methylene Blue Monograph for Professionals. [ONLINE] Available at:
https://www.drugs.com/monograph/methylene-blue.html. [Accessed 15 January 2019].

Kumar, N.. 2014. Impact of the Dye Industry on the Environment. [ONLINE] Available at:
https://www.slideshare.net/NehaKumar09/impact-of-the-dye-industry-on-the-
environment. [Accessed 15 January 2019].

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