Lost During First Extraction - help wanted

[Sakkadelic]

Are you bringing the solution to boiling or near boiling after adding the salt and letting it cool down from there?
How much salt per 100ml are you using?

You can always try reheating it and everything should dissolve, then let it cool down slowly in a bath of hot water undisturbed to get large needle crystals.

I hope you kept the decanted salt water.

Note that drying the manske harmalas from a pool of water like that will result in a significant salt contamination.

 

[its0x11]

Are you bringing the solution to boiling or near boiling after adding the salt and letting it cool down from there?
How much salt per 100ml are you using?

You can always try reheating it and everything should dissolve, then let it cool down slowly in a bath of hot water undisturbed to get large needle crystals.

I hope you kept the decanted salt water.

Note that drying the manske harmalas from a pool of water like that will result in a significant salt contamination.

I had the water hot and added it last night. The first time, I did boil it and got this result. I have the salted acid solution. I've kept everything just in case. I can put it together and boil it and then cool it again and see if crystals actually form this time.

 

[its0x11]

Oh and 10% salt, so I had 500ml of acidic solution, I added 60g of salt to 100ml of water and combined them

 

[Sakkadelic]

yeah I think it's worth a try. Heat it in a double boiler (outside water and solution at same level) once everything dissolves at near boiling, lightly cover the solution jar and leave it undisturbed until it reaches room temp.

I would up the salt concentration too, maybe 20%? I often go for near full saturation but that increases the salt contamination at the end so I try minimizing the water content before drying the harmalas, by using a coffee filter to collect the xtals and then pressing it gently between tissues to absorb the salty water.

 

[Sakkadelic]

You can also use the same settling trick to ease filtering. After observing the beauty of the xtlas, stir them and wait until they settle at the bottom, then decant and only pour the xtals at the bottom through the filter.

 

[its0x11]

I've put it all back together, boiled it for a minute, ensured everything dissolved and it's back in the flask cooling now. Not sure what xtals are. I assume you mean the crystals that will form, just haven't heard that term before.

 

[Sakkadelic]

Yes xtals is often used here to refer to crystals.
It's a good sign that it all dissolved back, though it is looking rather dark, for me it is usually a yellow orange color.

 

[its0x11]

It's been yellow orange or brown every time I base and red every time I acidify

 

[doubledog]

Manske sometimes produces such sediment, it seems to be dependent on specific concentrations of alkaloids and salt. Imo it still works as a purification step.

 

[its0x11]

Manske sometimes produces such sediment, it seems to be dependent on specific concentrations of alkaloids and salt. Imo it still works as a purification step.

So this is the second manske, and the second time it only produced sediment. Does that essentially mean I need to simply make freebase from this batch? It seems like the freebase is working fine, but when I try to get the salts, it doesn't quite work as expected. I prefer the salts, but I suppose I can make the freebase this time and try for salts from the next batch with a different Tek maybe.

 

[its0x11]

Probably difficult to see in these images, but it looks like it's pretty much mostly crystals at this point. I'll drain and collect them tomorrow morning and see what the haul ended up being from this one. So to keep the salts, simply pour and filter, dry them, and then dissolve in water for my desired concentration right?