1.

0 INTRODUCTION

1.1 Background
Dye is a coloured substance which has affinity to bind with the substrate
where it is generally applied in aqueous solution and in order to improve the
fastness of the dye on the fibres , it may need a mordant (Sharma, Tiwari, &
Singh, 2012). Several type of dyes are such as synthetic dyes, acid dyes, basic
dyes, mordant dyes and reactive dyes (Sharma et al., 2012).

Dyes are widely used in textiles, rubber, plastics, printing , leather and
cosmetics industries to colour their products (Bharathi & Ramesh, 2013). The
continuous flow of dye will cause the nature to absorb sunlight strongly
causing the intensity of light absorbed by the water plants and phytoplankton
to decrease, which caused photosynthesis and dissolved oxygen of aquatic
ecosystem to reduce resulting in increasing in COD (Sharma et al., 2012).

Technologies used for removing dyes from industries effluents are such as
biological and physical methods which includes coagulation, electrochemical
oxidation, ion exchange, membrane separation and adsorption (Wong, Tan,
Abdullah, & Ong, 2009). The best way for decolorization or removal of dye is
through adsorption process, a surface phenomenon where adsorbate molecules
or ions in liquid or gas are concentrated on the surface of a solid (Ahmad et al.,
2014). Depending on the adsorption of the adsorbate on the adsorbate surface,
the process can be classified into Phys sorption or chemisorption (Ahmad et
al., 2014). Removal of dye through adsorption usually used activated carbon,
low-cost adsorbent , nanoparticulate adsorbent and other type of adsorbent
(Ahmad et al., 2014).

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 In most industries practice, waste water will be produced as a byproduct
which will result in water pollution. Dye removal from textile effluents has
been given much attention in the last few years as dye has the potential to
expose hazards to the environment with the presence of many toxicated
organic residues, acids, bases and inorganic contaminants (Chequer et al.,
2013). This will surely interrupt the natural equilibrium and affect the aquatic
food chain and aquatic life. In other words, it affects the whole ecosystem and
environment. The use of activated carbon also will result in the increment of
overall operating for dye removal.

In short, the experiment reports on factors that affect the removal of dye.
Thus, the main purpose of this experiment is to analyse the kinetic behaviour
of wastewater during adsorption process and identify the relation between the
mass of absorbent and concentration of dye.

1.2 Objectives
 To analyse the kinetic behaviour of the adsorption
 To test the adsorption behaviour of mango seed under with different
adsorbent dosage applied and initial concentration of dye use

1.3 Experimental Scope

In this experiment, mango seed was used as an adsorbent and methylene
blue was chosen as the dye solution. The mango seed was first collected,
washed, dried and grounded. For the first part of experiment, the methylene
blue is calibrated at different concentration of 10 mg/L, 20mg /L, 30mg/L
and 40mg/L. After that, the prepared methylene blue solution with
concentration of 20 mg/L and 40 mg/L were mix with different dosages of
adsorbent (0.3 g, 0.6 g and 0.9 g) with contact time of 15 minutes. The
sample solution from each part of the experiment was then withdrawn and
separated from the adsorbent and was centrifuged. The absorbance and

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 final concentration of supernatant solution was analyzed by using UV –
VIS spectrophotometer.

2.0 LITERATURE REVIEW

2.1 Selection of adsorbent

Adsorption has been found to be an important technology for the removal of dye
from waste water. Activated carbons are well known adsorbents with high surface area
but their high cost limits their large scale application. Thus, there is need for a low cost
and easily available adsorbents for the removal of dyes from the aqueous coloured
effluents.

Selection of the adsorbent for the development of low cost adsorbents depends
upon many factors. The adsorbent should be freely available, inexpensive and non-
hazardous in nature. Moreover, for good adsorption results, high contents of carbon or
oxygen in the adsorbent moiety are very necessary. Other characteristics include
high abrasion resistance, high thermal stability and small pore diameters, which results in
higher exposed surface area and, hence, high surface capacity for adsorption. A recent
study by Emeka Ndimele and S. Erendu (2018) mention that the adsorbents from natural
organic which is readily available and less expensive materials that have been used as an
adsorbent to achieve maximum absorption capacity. In this study, we used mango seed as
our adsorbent.

2.2 Selection of dye

There are different ways for classification of dye molecules. It can be classified in
terms of colour, structure or application methods. Due to the complexities of the colour
nomenclature from the chemical structure system, the classification in terms of application
is often favourable. The common dyes applied in the textile industry are acid dyes, basic
dyes, direct dyes, azo dyes, reactive dyes, mordant dyes, vat dyes, disperse dyes and sulfur
dyes, where azo derivatives are the major class of dyes that are used in the industry today.

Methylene blue is the most commonly used substance for dying cotton, wood and
silk. It can cause eye burns which may be responsible for permanent injury to the eyes of

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human and animals. On inhalation, it can give rise to short periods of rapid or difficult
breathing while ingestion through the mouth produces a burning sensation and may cause
nausea, vomiting, profuse sweating, mental confusion and methemoglobinemia
(Rafatullah et al., 2010). Therefore, the treatment of effluent containing such dye is of
interest due to its harmful impacts on receiving waters. In this experiment, Methylene blue
will be the adsorbent.

2.3 Testing Parameter

There are many factors will affect the adsorption of dye molecules such as solution
pH, initial dye concentration, adsorbent dosage and temperature. In-depth study and
optimisation of these parameters will greatly help in the development of industrial-scale
treatment process for the dye removal.

Effect of adsorbent dosage Adsorbent dosage is an important parameter in order

to determine the adsorbent’s capacity for a given amount of the adsorbate at the operating
conditions. In order to study the effect of adsorbent dosage on the adsorption process, it
can be carried out by prepare adsorbent-adsorbate solution with different amount of
adsorbents added to fixed initial dye concentration then shaken together until equilibrium
time. In our study, we manipulate the adsorbent dosage to investigate the kinetic behaviour
of the adsorption process.

Colour removal efficiency was determined for each concentration of wastewater

at fixed time interval (contact time). The dye removal percentage at equilibrium was
calculated by the following formula.

𝐶𝑜 −𝐶𝑒
Percentage of Dye Removal (%): × 100
𝐶𝑜

𝐶𝑜 −𝐶𝑒
Adsorption Capacities (𝑞𝑒 ): ×𝑉
𝑚

Where,
Co :Liquid-phase dye concentration at initial stage and

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Ce: Equilibrium stage respectively (mg/L);
V : Volume of dye solution (L) and m is the mass of adsorbent (g)

3.0 METHODOLOGY
3.1 Materials
5 g of dried Mango seed, 60 mg of methylene blue (MB) and distilled water.
3.2 Apparatus
250-mL Erlenmeyer flasks, 25 mL beaker, 50 mL measuring cylinder, 500
mL beaker, strainer, filter paper, Pestle and Mortar, Weighing Balance,
Spatula
3.3 Equipment
Magnetic Stirrer, MiniScan EZ 4500L

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 3.4 Procedure

3.4.1 Preparation and calibration of synthetic dye wastewater

Step 1: Dye Stock solution was prepared by dissolving accurately weighed dye in distilled water to
a concentration of 500 mg/L.

Step 2: The stock solution is diluted to 10 mg/L, 20 mg/L, 30 mg/L, 40 mg/L to prepare the dye
solution.

Step 3: The synthetic wastewater was centrifuged at 700 rpm for 10 minutes.

Step 4: The concentration of dye was analyzed through UV-VIS Spectrophotometer.

3.4.2 Preparation of adsorbent

Step 1: The mango seed is washed for several times to remove the dust impurity.

Step 2: The mango seed is dried under the sun for 4 days.

Step 3: The dried mango seed is stored in an air tight plastic container.

Step 4: The outer shell of the mango seed was shredded using sandpaper.

Step 5: 5g of absorbant sample was collected.

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3.4.3 Test of the effect of different concentration of dye and adsorbent dose

Step 1: 20 mg/L, 40 mg/L, 60mg/L of methylene blue solution are added into each
conical flask containing 0.3 g absorbent respectively and shake constantly.

Step 2: The sample solution was withdrawed after 15 min contact time for the colour
removal analysis.

Step 3: All samples are withdrawed from conical flasks and separate the methylene
blue solution from the adsorbent by filtration.

Step 4: The L, a, b values were measured using theMiniScan EZ 4500L and the
readings were recorded.

Step 5: Repeat step 1 until 4 with introduction of 0.6 g and 0.9 of adsorbent

Step 6: All the result and data are recorded into the tables.

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4.0 EXPERIMENTAL PLAN
4.1 Variables involved

In this experiment, there are some variables involved, which are identified as follows:

Table 1: Variable involved in this experiment

Variable Parameter

Amount of adsorbent used, g

Manipulated Variable (MV)
Initial concentration of the methylene blue, mg/L

Process Variable (PV) Absorbance of the methylene blue

Controlled Variable (CV) Final concentration of the methylene blue, mg/L

Contact Time, s

Fixed Variable Stirring Speed, rpm

Heating Temperature, ͦ C

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4.2 Timeline

In order to accomplish and achieve the objective of this experiment, team plan has been
drafted as below:

Table 2: Team plan to accomplish the experiment

Date Details

18th February 2019 Briefing and discussion with group members about their
respective parts. Distribute task to each group’s members.

18th February 2019 - Preparation of proposal.

26th February 2019

27th February 2019 Submission of proposal to Dr. Mariam for further verification.

7th March 2019 Presentation of proposal with Dr. Mariam.

12th March 2019 Conduct the dye removal experiment.

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4.3 Task Delegation

Table 3: Task distributed for every group member

Time Details

Before experiment Introduction: Husna Filzah Binti Ismail

Literature Review: Ahmad Amir Bin AB Qais

Methodology: Nurin Syahirah Binti Anwar

Experiment Plan: Jee Jap Haw

Anticipated Results and Discussion: Priyana Balasundram

Reference collection: All group members.

During experiment Data recording and observation: Jee Jap Haw & Husna Filzah Binti Ismail

Procedure Instructor: Priyana Balasundram & Nurin Syahirah Binti Anwar

Handling Equipment: Ahmad Amir Bin AB Qais

After experiment Cleaning Process: All group members

Results discussion: All group members
Report preparation: All group members (Individual report)

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5.0 ANTICIPATED RESULTS AND DISCUSSION
5.1 Tabulation of Data

Table 4: Absorbance with different initial concentration of methylene blue

Initial Concentration of Absorbance at 668 nm

Methylene Blue, (mg/L)
10
20
30
40

Table 5: Tabulated Data for Adsorption Kinetic Analysis

Amount Absorbance Initial Final Percentage Adsorption

Absorbent, Concentration Concentration Removal, Capacity
(g) (mg/L) (mg/L) (%)
20
0.3
40

20
0.6
40

20
0.9
40

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 Figure 1: Calibration curve of absorbance against concentration of methylene blue

Graph of Absorbance against Concentration of Methylene Blue

Dye Solution
Absorbance

0 10 20 30 40
Concentration of Methylene Blue Solution (mg/L)

Figure 2: Expected Percentage of dye removal using 0.3 g, 0.6 and 0.9 g with different
concentration of methylene blue

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 Percentage of Dye Removal against initial concentration of different
absorbent dosage

Percentage of Dye Removal, %

20 40
Initial Concentration of Methylene Blue Solution (mg/L)

0.3 g 0.6 g 0.9 g

5.2 Discussion
Figure 3: Absorption curve of Methylene Blue

Wavelength (nm)

Based on the analysis of the dye done by Sogbochi, Balogoun, Dossa and
Sohounhloue (2017), when determining the absorbance of methylene blue as a function
of wavelength, a peak was observed at a wavelength between 660 nm and 670 nm (Figure
3). Therefore, the maximum absorption wavelength (λmax) 668 nm to perform the
spectrophotometric analyzes of the solutions of methylene blue.

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 When determining the absorbance of methylene blue as a function of wavelength,
a peak was observed at a wavelength between 660 nm and 670 nm .We have therefore
chosen as the maximum absorption wavelength (λmax) 665 nm to perform the
spectrophotometric analyzes of the solutions of methylene blue. The calibration curve is
established from the dilution of methylene blue with 10 mg/ L, 20 mg/L, 30 mg/L and 40
mg/L.
According to Beer’s Lamber Law, if the type of substance and the path length are
constant, the absorbance is directly proportional to the concentration (in molarity) of the
substance in the solution, which indicated that higher absorption process will take place.
With increased initial dye concentration, the dye removal percentage is expected
to decrease. This is mainly due to the saturation of adsorption sites on the adsorbent
surface. At lower concentration, unoccupied actives sites on the adsorbent. On the other
hand, the percentage of dye removal is expected to increase with increasing adsorbent
dosage, where the number of sorption sites at the adsorbent surface increases by increasing
the dose of the adsorbent and give us a result in increasing the percentage of dye removal
from the solution.

6.0 Reference

Sharma, N., Tiwari, D. P., & Singh, S. K. (2012). Decolourisation of Synthetic Dyes by
Agricultural Waste- A Review. International Journal of Scientific & Engineering
Research, 3(2).
Ahmad, A., Setapar, S. H. M., Chuong, C. S., Khatoon, A., Wani, W. A., Kumar, R., &
Rafatullah, M. (2014). Recent Advances In New Generation Dye Removal
Technologies. RSC Advanced(5). doi: 10.1039/c4ra16959j

Chequer, F.M., Rodrigues, G.A., Anastacio, E.R., Cardoso, J.C., Zanoni, M.V., & Palma,
D.P. (2013). Textile Dyes: Dyeing Process and Environmental Impact. Retrieved
from http://dx.doi.org/10.5772/53659

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Bharathi, K. S., & Ramesh, S. T. (2013). Removal of Dyes Using Agricultural Waste as
Low-Cost Adsorbents: A Review. Applied Water Science, 3, 773-790. doi:
10.1007/s13201-013-0117-y
Wong, S. Y., Tan, Y. P., Abdullah, A. H., a Ong, S. T. (2009). The Removal of Basic and
Reactive Dyes Using Quartenised Sugar Cane Bagasse Journal of Physical
Science, 20(1), 59-74.

Rafatullah, M., Sulaiman, O., Hashim, R. & Ahmad, A. (2010). Adsorption of methylene
blue on low- cost adsorbents: a review Journal of Hazardous Materials, 177(1-3),
70-80. Retrieved from doi.org/10.1016/j.jhazmat.2009.12.047

Emeka Ndimele, P. and S. Erendu, E. (2018). Chapter 24 – Remediation of Crude Oil.

The political Ecology of Oil and Gas Activities in Nigerian Aquatic Ecosystem,
369-384. Retrieved from doi.org/10.1016/B978-0-12-809399-3.00024-0

Sogbochi, E., Balogoun, C.K., Dossa, C.P.A., Sohounhloue, D.C.K. (2017). Evaluation
of Adsorption Capacity of Methylene Blue in Aqueous Medium by Two
Adsorbents: The Raw Hull of Lophira Lanceolata and Its Activated Carbon,
American Journal of Physical Chemistry, 6(5), 76-87. Retrieved from doi:
10.11648/j.ajpc.20170605.11

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