Syrian Rue Extraction going well and then nothing

[DreadyMofo]

Hi,

Just a quickie here. Was cleaning up my extraction with another vinegar/water/salt. So had the Harmala freebase and dissolved in the acidfied water and then added salt (or did I)? Left it overnight to precipitate out and there was nothing there at all in the morning?

In the rush to get to work for some reason I addde more sodium carbonate and it fizzed up quite furioussly to see if it would change colour back to the freebase. Now I am thinking I must have forgotten to salt it. Now I am home there is something in there and presumme this is the freebase again and I can repeat as before.

Am gutted as it was looking great.

Any advice please )

 

[endlessness]

Advice 1: Dont extract while so stoned (or take notes if youre a forgetful person)

Advice 2: Add more sodium carbonate to see if more base precipitates, decant/filter to retrieve alkaloids, and repeat process as desired.

 

[DreadyMofo]

Thank you Endlessness... will perhaps take notes next time... I think I got confused because I had two extracts going on at the same time as I couldn't grind up my seeds too well. I decided to let the remaining seeds sit in a strong vinegar/water solution for a couple of days and do another run on that one. So at the time I had the first batch in salt form and the new batch in freebase and turning it to salts (which it now has) and then based and (forgot to) salt the original. The plan was I would have both batchs in salt form and to mix them together and continue cleaning my poduct. The smoke probably didn't help any either...

So how much more soduim should I add. What has sunk to the bottom seeems a lot less than what I use to have. Also isn't my solution very acidic as it is 3:1 vinegar to water. I guess too much is better than too little.

I feel I have gone one step forward and 5 back! Oops

 

[endlessness]

The fizzing/bubbling when you add the sodium carbonate is the sodium carbonate reacting with the vinegar, making the solution less and less acidic. If you added just a bit, its probably still acidic, and what you have on the bottom is some precipitated inactive gunk. If you added more, it became neutral/basic and might be some alkaloids are there too. If you added enough, all alkaloids precipitated. Since you didnt measure the pH, its impossible to know. Just add some more sodium carbonate (or sodium carbonate saturated solution) and see if it still fizzes/changes color, and keep adding till it stops changing color. Then retrieve crystals.

Good luck

 

[DreadyMofo]

I just found some litmus papers I had lying around and checked the pH and it was neutral so added some more sodium carbonate and now it is definetly alkaline and a lot is precipitating out. However in the process it didn't really change colour, the freebase started forming pretty much immediately and I feel I am back on track.

Just one last question though, will everything be just as clean as ti was before? I had some lovely needles growing last time )

Ta

 

[endlessness]

Doesnt matter much, if its dirty, redissolve, filter, reprecipitate...

But I dont think it can have gotten dirtier if you didnt add any dirt..

 

[DreadyMofo]

well it was just off white last time and now it is back to orange ( as you say though just got to go through the process again. I did add a lot of sodium carbonate to get it back to this. Could that have effected anything? On the plus side, have just filtered the second freebase batch and is lovely and pale. Think I'll add them together now and go about cleaning it all up )

Thanks for advice

 

[DreadyMofo]

last question on this one, I just redisolved everything in 3 parts vinegar to 1 part water (about 300ml in total) and added 38g salt and after about a minute it started precipitating. Previously the first signs of crystals forming took about 2 hours; just before I put it in the fridge. How come it's precipiting so quickly all of a sudden, or was my previous attempts extremely slow? Also I am certain I have lost a lot of product along the way. What kind of yield should I expect from 50g Syrian Rue seeds?

Thank you

 

[endlessness]

why would you have loss yield unless you threw something away? unless you didnt add enough sodium carb before or something.

Also notice its normal to lose some weight during each reprecipitation because youre cleaning up your harmalas...

As for why the quick precipitation, because you added too much salt. 100g per 1l, so 30g salt for 300ml liquid.. if you add more, it precipitates faster. Also you should add salt while whole mix is boiling, and let it cool slowly.

As for yield, between 0.5-5% depending on your seeds, potential losses during process and how clean you make them.

 

[evil804]

edit - endless already said it. too much salt.

ive been getting 4% dry weight of light tan harmalas from going acid/base/manske/base/manske/base. base your water after the second manske, i have found manske only precips out 85% or so of the harmalas. my last go i had 6 grams or so of harmalas after my final manske, and based that water to retrieve another gram.

 

[Kryll]

nvm