rombusempire
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This is how I prepared it including areas where I believe may have been the culprit for the murkiness:
1) pellets from 4 carts were dissolved in methanol for 1 hour while constantly crushed.
2) The solution was then filtered using a fisherman's hat (hat filter). The solution was still murky after the filter. IN a previous attempt, I used a 0.45micron whatman filter tpo filter teh binders and the solution was very very clear, but I had to use at least 10 such filters (it was impssible to push more than 5mL of fluid through it).
3) 2g of Caustic Soda pellets (pure NaOH) were dissolved in approx 3mL of hot water. The pellets dissolved perfectly.
4) Caustic soda solution was added to the methanol solution and left in the freezer for 1 hour.
5) 400mL of pre-chilled boiled water (not distilled) was added drip wise to teh solution in the freezer.
6) The solution turned milky white wiht a tinge of bright green. The solutin was filtered using coffee filter (brown paper)
7) Another 400mL of prechilled boiled water was added (quickjly this time) to the filtrate. MOre crystals formed, and those too were collected using coffeee filter.
8) The crystals were consolidated and washed with approx 1L of prechilled boiled water through the hat filter.
9) The hat filter and the crystals on top were put in an oven and baked for 3 hours at 85 degrees celsius.
10) The remaining dried powder (approx 5g) was placed in a 150mL beaker. Grapeseed oil (8mL) was added to it. The powder woudl not dissolve.
11) The oily powder was then placed in the oven at 125 degrees celsius for 1 hour. I did this so that the crystals would melt and hence, dissolve. They would not dissolve at lesser temperatures.
12) 3mL of Benzyl alcohol was added to the oily solution.
13) The oily solution could not be pushed through the whatman 0.45 syringe prefilter (only an initial few drops can be pushed through).
Do you know what is going on?
** the previous attempt, I used 1 cart and the 0.45 whatman filter to filter the binders at the first step. It was still almost impossible to push the oily solution through the .45 micron filter at the end.
1) pellets from 4 carts were dissolved in methanol for 1 hour while constantly crushed.
2) The solution was then filtered using a fisherman's hat (hat filter). The solution was still murky after the filter. IN a previous attempt, I used a 0.45micron whatman filter tpo filter teh binders and the solution was very very clear, but I had to use at least 10 such filters (it was impssible to push more than 5mL of fluid through it).
3) 2g of Caustic Soda pellets (pure NaOH) were dissolved in approx 3mL of hot water. The pellets dissolved perfectly.
4) Caustic soda solution was added to the methanol solution and left in the freezer for 1 hour.
5) 400mL of pre-chilled boiled water (not distilled) was added drip wise to teh solution in the freezer.
6) The solution turned milky white wiht a tinge of bright green. The solutin was filtered using coffee filter (brown paper)
7) Another 400mL of prechilled boiled water was added (quickjly this time) to the filtrate. MOre crystals formed, and those too were collected using coffeee filter.
8) The crystals were consolidated and washed with approx 1L of prechilled boiled water through the hat filter.
9) The hat filter and the crystals on top were put in an oven and baked for 3 hours at 85 degrees celsius.
10) The remaining dried powder (approx 5g) was placed in a 150mL beaker. Grapeseed oil (8mL) was added to it. The powder woudl not dissolve.
11) The oily powder was then placed in the oven at 125 degrees celsius for 1 hour. I did this so that the crystals would melt and hence, dissolve. They would not dissolve at lesser temperatures.
12) 3mL of Benzyl alcohol was added to the oily solution.
13) The oily solution could not be pushed through the whatman 0.45 syringe prefilter (only an initial few drops can be pushed through).
Do you know what is going on?
** the previous attempt, I used 1 cart and the 0.45 whatman filter to filter the binders at the first step. It was still almost impossible to push the oily solution through the .45 micron filter at the end.
