Help with Manske precip of Harmalas

[Gone-and-Back]

Last night I conducted the manske extraction on syrian rue. I let this sit in the fridge for 8 hours to cool off, and when I came back it was as cold as it could of been from sitting in there.

I used a quarter pound of syrian rue seeds, and got what looks like a very small amount of alks that precipitated out. They are currently under a fan to dry. However, the water that is left over after straining everything out looks to be saturated with more harmala alks, because it is still a deep red color. Is this color the remaining Harmalas, or is this due to the other alks that are present in the rue, but didnt precip out during the cooling process?

If it is indeed more harmalas, would the heating of the liquid and another salt water addition done bring about more of the harmala alks? This is how the water looks still after the solution was poured through a cloth to collect the solids.

 

[Gone-and-Back]

I filtered out everything that I can, and am going to be saving the liquid for now incase someone mentions a way to get more alks out. I plan on freebasing these alks, and wanted to use sodium carbonate as the base agent, but can I clean the alks using a sodium carbonate solution the same as I would with lye or ammonia? Or will this process only work with lye and ammonia? I know they can be freebased with the sodium carbonate, but I dont know if this can be done over and over to wash/clean the final product. Advice would be appreciated.

 

[Gone-and-Back]

I decided to heat up the water and do another salt addition. There are a lot more alks that have crashed out, and it looks much more sparkly then the last batch did, which yielded a small amount of light brownish material with a very small portion of sparkling crystals.

However, I did do the rest of the procedure on what I did get from the first run. When added to the alcohol, (Isopropyl, because I dont have access to ethyl or methyl alcohol), the crystals dissolved into the IPA, and the rest of the brownish dirt looking stuff did not. I then filtered and kept the alcohol and threw away the solids. This solution was held up to a black light, and it glowed very brightly indicating a high concentration of alks.

The solution was then evaped onto a pyrex pan, and the resulting crystals were then scraped up and saved. There was a very tiny amount of the crystals, however I do not know how much exactly due to my lack of a scale currently. So this showed that the process was done correctly so far. However, when I went to redissolve the alks into an acidified water solution to then add my bass agent, sodium carbonate, that I ran into a problem.

The sodium carbonate readily dissolved and reacted forming a bunch of bubbles. There was a brown solid that formed and floated to the top, only a very small amount though. There was a white solid that appeared to form on the bottom, however I feared that this was just the sodium carbonate since there was no indication of color change that usually occurs with freebasing something. The solution remained the same color.

I still have my second jar of alks sitting in the fridge, I decided to let it settle for 24 hours to see if that increases the amount that crashes out. I may put it in the freezer for half an hour to an hour to further reduce the temp and get everything out that I can, without freezing it of course. However, when I get back down to the freebasing, what did I do wrong that I should fix this time? Im thinking Im just going to go with ammonia or lye to freebase it originally, then redissolve it in a solvent and evap again and again until I feel there is no more lye or ammonia left behind. Would this be a good method?

 

[Gone-and-Back]

I really could use some help here guys...

 

[Vodsel]

Ok, I'm a little lost regarding where you are now exactly, but a few comments for starters.

Sodium carbonate works perfectly fine. Just keep in mind that, as you start adding it slowly to the acidified alkaloids solution, it will react with the vinegar and release a fair amount of gas - hence the bubbling. That is normal, and if you keep adding small amounts of sodium carbonate and stirring, eventually all the acetate ions will react and the solution will stop bubbling. That's when you will start getting precipitates with further SC addition. And whether you add SC as a solid or a saturated SC solution, the result will be the same. It may be a good idea to use saturated water in the final basing, to make sure that no SC solid salts will be left behind along with the freebase harmalas as you filter.

And about manske, if you get only partial precipitates it's most likely a sign that the solution was not enough saturated with salt. And when you filter out the liquid after manske, a cloth might not be fine enough.

Am I being helpful, or missing your key question right now?

 

[Gone-and-Back]

That helps a lot, thank you. Right now I am at the point where I have evaporated the alcohol and am left with a fine tanish brown powder that is very sparkly and crystal looking. A friend tested about 20mg placed under the tongue for a min or two. Effects were noticed for sure, as the amount of mj that she smoked afterwards got her a lot more stoned then it usually does. Also some coordination issues and slight drowsiness.

So to freebase them I have to put them back into a solution. Should I just use water saturated with vinegar? Or dissolve them in straight vinegar? When I add the SC I'm most likely going to saturate water with it like you suggested and add that to the harmala solution drop by drop.

Also, I was told that you can get SC by the simple process of heating up baking soda in the oven for long enough. Is this true?

Also, the container that I was saying is in the fridge has been sitting there this whole time and has developed a pretty thick layer of sediment on the bottom of it. Is this all harmala HCL salts? Or by this point is most of that just salt and other junk?

 

[Vodsel]

So to freebase them I have to put them back into a solution. Should I just use water saturated with vinegar? Or dissolve them in straight vinegar?

The alkaloids precipitating with manske are chlorhydrates. That means you can redissolve them in plain distilled water, no vinegar needed.

When I add the SC I'm most likely going to saturate water with it like you suggested and add that to the harmala solution drop by drop.

No need to go drop by drop, you can pour slowly until no more color change occurs. Any excess of SC water will be filtered out leaving the freebase harmalas behind. You might go drop by drop if you are using a super-saturated hot SC solution. In that case, and since the SC solubility in water will decrease as the solution cools off, some SC might precipitate and mix with the harmalas. But if you are doing the whole freebasing at ambient temperature, no need to be extremely careful with the amount of SC water added.

Also, I was told that you can get SC by the simple process of heating up baking soda in the oven for long enough. Is this true?

True. I don't remember exactly the temperature and time since I've never done this, but it should be easy to find with a search.

Also, the container that I was saying is in the fridge has been sitting there this whole time and has developed a pretty thick layer of sediment on the bottom of it. Is this all harmala HCL salts? Or by this point is most of that just salt and other junk?

Salt should crash only if the solution was super saturated before chilled. Other unwanted stuff (vasicine, deoxyvasicine and vasicinone) might still be there if you have only performed once the manske. Check again the Harmalas Extraction and Separation Guide, it's very comprehensive and will answer any doubts.

 

[Gone-and-Back]

Thank you very much, I appreciate that someone could finally help me out with this. Regarding that solution thats in the fridge, could I just filter it out and dissolve in alcohol, then filter out the remaining solids to have another harmala/alcohol solution? Or would this contain other unwanted alks as well?

 

[Vodsel]

That depends on how pure you want your harmalas to be. If manske has been performed only once in that solution, chances are there will still be a significant amount of the other alkaloids. If you don't mind them being there, you can just filter solids out, dissolve them and proceed as you want. But if you want to purify your harmalas, those solids should be redissolved in water, re-basified and re-manskeed. Again, the guide will explain it better than I do.