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1. Summery of method
This method describes the determination of SO2 according to the modified Monier – Williams
method. It involves the acidification of a sample, followed by the distillation of SO2 (with
Nitrogen Gas) out of the sample in to a hydrogen peroxide solution. The SO2 and hydrogen
peroxide reacts to form H2SO4 according to the following reaction:
This weak acid is then titrated with Sodium hydroxide till a end point is reached.
2. Apparatus
2.1. SO2 Distillation apparatus figure 1.
2.2. Volumetric flask 1lt × 3.
2.3. Volumetric flask 500ml × 2.
2.4. Volumetric flask 100ml × 2.
2.5. Amber reagent bottle × 2.
2.6. Pipette volumetric 15ml.
2.7. Pipette volumetric 10ml.
2.8. Pipette volumetric 50ml.
2.9. Dropper.
2.10. Scale 2 decimal (0.00g)
2.11. Heating mantle / Bunsen burner.
2.12. N2 Cylinder with regulator and fittings for 5mm ID pipe.
2.13. Water connection, with constant water flow and fittings for 5mm ID pipe.
2.14. Dr Schillings Burette 50ml.
2.15. Magnetic stirrer (Optional)
2.16. Wash Bottle 500ml.
2.17. Beaker 250ml.
2.18. Funnel 35mm
2.19. Cylinder 100ml.
2.20. Tubing
3. Chemicals
5. Methodology
5.1. VERY IMPORTANT! Before preparing distillation flask (4) the distillation receiver
must be prepared as follow: To the distillation receiver (7) 15ml 0.6% H2O2 (Hydrogen
peroxide) solution is added and 60ml distilled or deionized water using the 100ml
cylinder. Add to the mixture a few drops of indicator. The solution will turn blue. Add
then a few drops of the 0.01N NaOH (sodium hydroxide) solution to the mixture until it
turns light green.
5.2. The N2 wash bottle is prepared by adding 0.1N NaOH solution to it.
5.3. Add 15ml of 85% Orthophosphoric acid to the dropping funnel. (4.2)
5.4. Prepare the distillation flask (4) by placing 15g ± 1g of sample, 50ml methanol and 50ml
of distilled water into the flask.
5.5. Connect the distillation flask to the apparatus. Insert the N2 injector (4.1) and dropping
funnel (4.2) containing the phosphoric acid into the distillation flask (4).
5.6. Open the stop cock on the dropping funnel (4.2) so that the phosphoric acid flows into
the distillation flask (4).
5.7. Ensure the tap water to the system is opened and has a constant flow.
5.8. Open the N2 stream to the system (c.a. ±60 bubbles/min)
5.9. The liquid in the distillation flask is heated to boiling by a burner or heating mantle and
then held at a gentle boil.
5.10. The time of distillation, including heating up period should take approximately
15 min.
5.14. Calculation:
1ml 0.01N NaOH represents 0.32mg SO2
3. Wash Bottle
3.1 Wash bottle head
4. Distillation flask
4.1 N2 injector
4.2 Dropping funnel
5. Splash head
6. Reflux condenser
6.1 Stopper
7. Receiver flask
7.1 Gas inlet tube
8. Control bottle
(optional)
8.1 Control bottle head
Figure 1