STANDARD OPERATING PROCEDURE

SP # APM008

Version:
1.0
Replaces:
N/A
Page 1 of 6
Date:
21/07/2010
Revise by: 21/07/2013
Advanced Porous Materials Laboratory, School of Chemistry, The

Written by:
Xingdong Wang
Reviewed by: Dana Morgan
Authorised by: Rachel A.
Caruso
University of Melbourne

USE OF PHOTOCATALYSIS SETUP

1.

Introduction
This SOP sets out the procedure for the use of the photocatalysis setup. A photocatalysis
setup is used for the assessing the photocatalytic activity of photoactive materials, in term
of the degradation of an organic pollutant in water. It includes a power station, a 500 Watt
Hg-Xe globe, a circulating water bath (cooling), an O 2 bubble system and a reaction
chamber with stirrer bar.

2.

Scope
This procedure applies to all staff, students and visitors of the Advanced Porous Materials
Group in the School of Chemistry at the University of Melbourne that work in the
laboratory and have the potential to use the photocatalysis setup.

3.

Safety
The usual safety concerns involved with general laboratory working procedures,
electrical instruments and gas cylinders must be observed. Additionally, extra care should
be taken to minimise the risks of UV burns on the skin and damage to the operators eyes.
Personal protective equipment (PPE) including safety glasses or face shield, and
laboratory coat and gloves must be worn when handling UV light.
Avoid wear UV light safety goggles to avoid irradiating the eye with UV light.
The light-blocking fume hood sash must be lowered during experimental runs to
minimise UV irradiation of the laboratory environs and personnel.
The UV light must be turned off immediately after completing the experimental run at
the control panel. Then, switch off the control panel once the system has cooled
down, indicated by the fan stopping.

4.

Licences and Permits

N/A

5.

Training and Competency

The trainee must have already mastered an understanding of and have been given the
instruction in the use of the photocatalytic apparatus by the instrument supervisor.
Competency will be assessed by close observation of the trainee by the instrument
supervisor or an approved trainer. The training and competency records are to be filed
and stored in the Advanced Porous Materials Laboratory Safety Folder.

STANDARD OPERATING PROCEDURE

SP # APM008

Version:
1.0
Replaces:
N/A
Page 2 of 6
Date:
21/07/2010
Revise by: 21/07/2013
Advanced Porous Materials Laboratory, School of Chemistry, The

6.

Written by:
Xingdong Wang
Reviewed by: Dana Morgan
Authorised by: Rachel A.
Caruso
University of Melbourne

Risk Assessments
Refer to the following risk assessment forms:
Use of photocatalysis setup, assessed 29/07/10.
Use of UV lamps, assessed 02/02/10.
Use of electrically operated equipment, assessed 20/06/07.
Use of microcentrifuge, assessed 27/07/10.
Class 2.2 dangerous goods non-toxic, non-flammable compressed gasses, assessed
09/11/09
Moving full and empty gas cylinders, assessed 31/07/09.
Waste solvent disposal, assessed 09/11/09.

7.

Equipment and Maintenance / Handling and Storage / Labelling

8.

The entire apparatus must be assembled in a fume hood to ensure adequate

ventilation.
The fume hood environs and apparatus should always be kept dust-free.
The condition of the unit and electrical cord/plug must be inspected prior to use.
Equipment deemed to be unsafe is to be removed from service immediately.
Replacement of the UV globe is restricted to a qualified electrician.
Replacement of the optical filter is restricted to the instrument supervisor.
The waste solution must be disposed of in the appropriate waste receptacle.

Operating Procedures
Methylene Blue (MB) degradation reaction:
Reaction preparation:
1. Prepare a test solution (160 mL) with photocatalyst concentration of 0.5 g/L (UV
light, 0.08 g) or 1 g/L (visible light, 0.16 g). The initial concentration of MB should
be around 50 mg/L for UV and 12.5 mg/L for visible light.
Adsorption test (0 min):
1. Prepare the sample in the dark and stir with a magnetic slug for the required time
(preferably overnight).
2. Then, subsample a 1 mL aliquot and centrifuge for 10 minutes using a
microcentrifuge (Hermler Z 233 M-2) at 15000 rpm.
3. Dilute the supernatant (0.8 mL) with deionised water (1.6 mL).
4. Transfer diluted adsorption test sample into a cuvette and analyse the Vis spectrum
(400800 nm) on the Cary 50 Bio UV-Vis spectrometer.
Photocatalytic test:

STANDARD OPERATING PROCEDURE

SP # APM008

Version:
1.0
Replaces:
N/A
Page 3 of 6
Date:
21/07/2010
Revise by: 21/07/2013
Advanced Porous Materials Laboratory, School of Chemistry, The

Written by:
Xingdong Wang
Reviewed by: Dana Morgan
Authorised by: Rachel A.
Caruso
University of Melbourne

1. Open the tap of the running water system slightly, then switch on the water
circulation system. Allow the water to cool the reaction chamber and liquid filter,
respectively and allow to equilibrate.
2. Gently open the regulator of the gas cylinder until a flow rate of 1.5 mL min-1 is
attained. This should appear as a gentle bubbling of air through the reaction solution.
This flow rate should be maintained throughout the entire experimental run. Place the
gas outlet and a thermometer into the reaction chamber.
3. Turn on the lamp system and allow it to warm up and equilibrate over a 30 minute
period. Use the metal light shield to block the light.
4. Pour the test solution into the reactor quickly and allow to stabilise with the gas
flowing for 20 minutes.
5. Shine the light on solutions in the reaction chambers by removing the metal light
shield. Subsample 1 mL of the reaction mixture using a plastic transfer pipette at
intervals of 15, 30, 45 and 60 min for UV light and at 30, 60, 90 and 120 min for
visible light.
6. Centrifuge the 1 mL aliquots for 10 minutes using a microcentrifuge (Hermler Z 233
M-2) at 15000 rpm.
7. Dilute the supernatant (0.8 mL) with deionised water (1.6 mL).
8. Transfer diluted adsorption test sample into a cuvette and analyse the Vis spectrum
(400800 nm) on the Cary 50 Bio UV-Vis spectrometer.
9. When the photocatalysis experiments are complete, turn off the lamp (left hand
switch on the control panel). Allow the instrument to cool down (1015 min, when
the fan stops working) before turning off the main power.
Calibration:
1. Using a stock solution of MB (50 ppm) prepare 0, 2.5, 5, 7.5, 10 and 12.5 ppm stock
solutions.
2. Analyse the Vis spectrum (400800 nm) on the Cary 50 Bio UV-Vis spectrometer and
prepare a calibration curve.
Data analysis:
1. Calculate the concentration of un-reacted MB for all reaction intervals from the
calibration curve.
9.

Controls and Calibrations

The light intensity is monitored at semi-regular intervals, but especially when the light
source is changed between UV and visible light. A photocatalysis run of commercial
Degussa P25 is used as a benchmark.

10.

Waste Disposal

STANDARD OPERATING PROCEDURE

SP # APM008

Version:
1.0
Replaces:
N/A
Page 4 of 6
Date:
21/07/2010
Revise by: 21/07/2013
Advanced Porous Materials Laboratory, School of Chemistry, The

Written by:
Xingdong Wang
Reviewed by: Dana Morgan
Authorised by: Rachel A.
Caruso
University of Melbourne

Reaction waste solution: Waste reaction solution must be disposed of in the appropriate
waste container (e.g. water soluble waste solvent, water insoluble waste solvent,
halogenated waste solvent). Refer to relevant chemical MSDS before disposal.
Cleaning solution: Water used to clean the reaction chamber may be disposed of down the
sink.
11.

Relevant Documents / References

Standard Operating Procedures:
Use of microcentrifuge, Advanced Porous Materials Laboratory, School of Chemistry,
The University of Melbourne, Version 1.0, 27/07/10.
Risk assessments applicable to the SOP are listed in Section 6.

12.

Signage / Summaries / Templates

Competency Training Records Form Attached, see page 4.
Copies of this form are to be stored and filed and in the Advanced Porous Materials
Laboratory Safety Folder.

13.

Appended Material
N/A

STANDARD OPERATING PROCEDURE

SP # APM008

Version:
1.0
Replaces:
N/A
Page 5 of 6
Date:
21/07/2010
Revise by: 21/07/2013
Advanced Porous Materials Laboratory, School of Chemistry, The

Written by:
Xingdong Wang
Reviewed by: Dana Morgan
Authorised by: Rachel A.
Caruso
University of Melbourne

ADVANCED POROUS MATERIALS LABORATORY

COMPETENCY TRAINING RECORDS PHOTOCATALYSIS SETUP

Date

Name

University/Dept.

Trainer

Competency
Date

Trainee

Trainer

STANDARD OPERATING PROCEDURE

SP # APM008

Version:
1.0
Replaces:
N/A
Page 6 of 6
Date:
21/07/2010
Revise by: 21/07/2013
Advanced Porous Materials Laboratory, School of Chemistry, The

Written by:
Xingdong Wang
Reviewed by: Dana Morgan
Authorised by: Rachel A.
Caruso
University of Melbourne