Spirochete
Rising Star
Hello everyone,
Here is a pic of a colloidal layer under the aqueous layer. Is this normal? Here is the procedure so far:
Boil 90 g of powder in about 500 ml distilled water with 1 ml phosphoric acid added. The acid was only added to the first boil. After the 7th boil, the water did not take a green tint. The solution was filtered with a fine wire filter and then a cloth filter. The liquid was reasonably filtered but not well enough to pass through a coffee filter without clogging.
The solution was boiled down to about 1000 ml, and defatted with xylene. An emulsion layer was noted between the polar and non polar layers which resolved with a hot water bath and mild agitation. He would simply turn the separatory funnel 90 degrees and stop abruptly. Each time he could see layers of the emulsion falling into the solution. The reason he did not boil down the solution further is that it seems if the water has too much solute it would not behave in a predictable manner.
He plans on precipitating with HCl from the xylene layer so he added KOH to the solution until the pH was 12-13, and then added a small amount of xylene. Only a small amount was added because with a LogP of 0.78, only around 15% of the alkaloids will be in the xylene layer with each pull. He will do 6-7 pulls.
In the pic there is a colloidal layer at the bottom. It has a fluffy texture to it. It is currently being heated in a hot water bath. Is it normal to have this layer, and are any alks suspected to be in this layer? Is very fine filtration important with these mesc extrations as it is with the harmala manske teks?
Here is a pic of a colloidal layer under the aqueous layer. Is this normal? Here is the procedure so far:
Boil 90 g of powder in about 500 ml distilled water with 1 ml phosphoric acid added. The acid was only added to the first boil. After the 7th boil, the water did not take a green tint. The solution was filtered with a fine wire filter and then a cloth filter. The liquid was reasonably filtered but not well enough to pass through a coffee filter without clogging.
The solution was boiled down to about 1000 ml, and defatted with xylene. An emulsion layer was noted between the polar and non polar layers which resolved with a hot water bath and mild agitation. He would simply turn the separatory funnel 90 degrees and stop abruptly. Each time he could see layers of the emulsion falling into the solution. The reason he did not boil down the solution further is that it seems if the water has too much solute it would not behave in a predictable manner.
He plans on precipitating with HCl from the xylene layer so he added KOH to the solution until the pH was 12-13, and then added a small amount of xylene. Only a small amount was added because with a LogP of 0.78, only around 15% of the alkaloids will be in the xylene layer with each pull. He will do 6-7 pulls.
In the pic there is a colloidal layer at the bottom. It has a fluffy texture to it. It is currently being heated in a hot water bath. Is it normal to have this layer, and are any alks suspected to be in this layer? Is very fine filtration important with these mesc extrations as it is with the harmala manske teks?
