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Freshly prepared 0.1 M aqueous NaBH4 (0.6 mL) solution was added dropwise to this mixture under vigorous stirring.
After this time, the mixture was cooled to −5°C in an ice-salt mixture under vigorous stirring.
After 30 min of stirring, 10 mL of 1.2 M sodium acetate solution in EG was added to the previous mixture under vigorous stirring.
An aqueous solution of NaBH4 (0.2 M, 12.5 mL), cooled to 0 °C, was injected rapidly into the above mixture under vigorous stirring.
Briefly, under N2 purging, 1 g of FeCl2.4H2O and 2.6 g of FeCl3.6H2O were dissolved in 25 ml distilled water and kept at 75 °C for 10 min, then 10 mL of ammonia solution (25%%) was dropped into the above mixture under vigorous stirring and keeping at 75 °C for a further 1.5 h.
After 5 to 10 min, 10 mL fumed nitric acid was added slowly in 15 min. Then, graphite powder (1.0 g, with particle size <45 μm) was added into the mixture under vigorous stirring for 30 min with the flask held in the iced bath.
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The urea solution was added into the dodecylamine-TIP mixture solution under vigorous stirring at ambient temperature.
The mixture was left under vigorous stirring for 2 h.
This forms two phases, and the mixture was kept under vigorous stirring.
MSA (1795 mg) was dissolved in methanol (400 ml) and the mixture was kept under vigorous stirring in an ice bath.
The whole mixture was heated to 85 °C under vigorous stirring until the solution became clear.
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