Procedure for Fe2+/Fe3+ addition

Fe2+ reagent FeSO47H2O Iron (II) sulphate heptahydrate

Fe3+ Iron (III) chloride anhydrous (FeCl3)
K3[Fe(C2O4)3] potassium ferrioxalate
Iron (III) chloride hexahydrate (FeCl36H2O)
A.
1.
2.
3.
4.
5.

Experiment procedure
Set up the reactor according to Figure 1 illustrated above.
Connect the pump to the double-jacket reactor by using rubber tubing between them.
Weight 0.5 g of zinc oxide into weighing beaker before transfer it into reactor.
Weight the desired amount of Fe3+ / Fe2+ before transfer it into reactor.
Add 200ml of phenol solution (25ppm) to the double jacket reactor using a measuring
cylinder and switch on the magnetic stirrer.
6. Switch on the pump in order to make cooling water recycle through the reactor jacket
to keep the temperature of reactor constant at 25oC.
7. Switch on the stirrer, allowing reaction mixture to be stirred for 30min in the dark and

supply oxygen (99.9% purity) into the solution at constant flow rate of 40mL min1
to insure oxygen saturation. need it to provide oxygen for H2O2 generation
8.
9.
10.
11.
12.

Using a syringe to take 3mL mixed solution and filter it into HPLC vials.
Switch on the lamp to allow photocatalytic reaction to start.
At 30min, switch off the lamp and repeat step 7.
Repeat step 8 and 7 in every 30 min until 150min.
After photocatalysis experiment, switch off light, stop stirring, cooling water, store
samples, wash reactor with deionised water and put it in oven (80oC) for next time use
and take it out of oven with heat protective gloves after it has dried.
13. All chemicals should be moved from working area and be stored properly.
14. Make sure electrical powers and water are switched off.

Volume of suspension 1L

Light intensity
pH value monitor using pH meter
mixture (phenol) dissolve in distilled water before transfer to reactor and add TiO2
0.5g/L
Stir prepared aqueous suspension in ultrasound before irradiation
Stir reaction solution continuously with magnetic stirrer and supply oxygen (99.9% purity)
into the solution at constant flow rate

of 40mL min-1 to insure oxygen saturation nad maintain the temperature at 30C
Oxygen saturated