4.

Methods / Procedures

List of Chemicals:
1. Sodium Hydroxide (NaOH)
2. Hydrochloric Acid (HCl)
3. Methylene Blue Dye (MB)
4. N,N-dimethylformamide (DMF)

List of Apparatus and Equipment:

1. Fourier Transform Infrared Spectroscopy (FTIR)
2. Ultra Violet-visible Spectroscopy (UV-Vis)
3. Analytical Balance
4. Drying Oven
5. Beaker
6. Magnetic Stirrer
7. pH meter
8. Flourescent lamp

List of Materials:
1. Platinum (Pt) plate
2. Nickel (Ni) plate
 A. Preparation of membrane by using Plastic Bottle (PB) of Low-density
polythyelene solution.

i. Cut PB into pieces, wash it to remove impurities then is dried in the drying oven at
40oC.
ii. Add 100g of PB and immersed in 500ml of N,N-dimethylformamide into a 1000ml
beaker and stirred.
iii. Left for 24 hours to ensure the compound was fully mixed.

B. Preparation of electrolysis

i. 50ml of membrane solution is added to one-compartement cell fitted with a platinum

plate cathode (2 cm x 2 cm) and nickel plate anode (5 cm x 2 cm) with power supply
480 mA cm-2 under normal atmospheric conditions at room temperature.
ii. After electrolysis the was impregnated, the mixture was spread in a beaker which
contained distillation water to yield a layer thin film of membrane catalyst.
iii. Then, the thin film catalyt ready for characterization and photocatalytic testing.

C. Photocatalytic reaction

i. Add 50 ml of the catalyst in 10 mg/L of MB aqueous solution in a beaker.

ii. Next, The catalyst was tested for decolorization of MB using a batch photoreactor
system containing a flourescent lamp (Philips Lifemax TLD 18W/54 daylight, 13000
h, 6200 K, 280-315 nm emission) and magnetic stirrer.
iii. Irradiated under flourescent light at room temperture for 2 hours with costant stirring
(distance light and the reaction vessel is 15 cm).
iv. Then, use UV-vis spectrophotometer to measure the remaining MB concentration.
v. The decolorization percentage:
(C0 – Ct )
Decolorization (%) = x 100
C0
C0 Initial concentration
Ct Variable concentration
a. Preparation of Dye Solution
i. Prepare 10 ppm, 20 ppm, 30 ppm, 50 ppm, 70 ppm and 100 ppm dye solution
by mixing 0.01, 0.02, 0.03, 0.05, 0.07g and 0.10g dye Methylene Blue
respectively with 1L of distilled water in 1L beaker.

b. Effect of pH
i. The effect pH solution on dye removal is 3, 5, 7, 9 and 11 with initial
concentration of dye solution 20 ppm. The pH of the solution was adjusted using
0.1 M HCl or 0.1 M NaOH solutions.
ii. Suspended in 50 mL of 20 ppm dye solution that has different pH value
iii. The contact time is 5, 10, 15, 30 and 60 minutes.
iv. Collect the sampling for further evaluation.
v. Evaluate the extent of reduction by using UV-VIS spectrometer by measuring
the maximum absorbance at 586 nm using Perkin-Elmer Lambda 35 UV-
Visible spectrophotometer

c. Effect of Dosage
i. Mix 5 different weight 0.1 g, 0.2 g, 0.3 g, 0.4 g and 0.5 g of with 20 ppm dye
solution.
ii. The contact time is 5, 10, 15, 30 and 60 minutes
iii. Collect the sampling for further evaluation.
iv. Evaluate the extent of reduction by using UV-VIS spectrometer by measuring
the maximum absorbance at 586 nm using Perkin-Elmer Lambda 35 UV-
Visible spectrophotometer.

d. Effect of Initial Concentration

i. Mix with dye solution with the prepared different concentration 10, 20, 30, 50,
70 and 100 mg/L
ii. The contact time is 5, 10, 15, 30 and 60 minutes.
iii. Collect the sampling for further evaluation.
iv. Evaluate the extent of reduction by using UV-VIS spectrometer by measuring
the maximum absorbance at 586 nm using Perkin-Elmer Lambda 35 UV-
Visible spectrophotometer.