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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
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.
5.
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.
8.
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:
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.
10.
Waste Disposal
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.
12.
13.
Appended Material
N/A
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
Date
Name
University/Dept.
Trainer
Competency
Date
Trainee
Trainer
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