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Syrian Rue extraction question - sodium carbonate sediment Options
 
ChaseTheRabbit
#1 Posted : 6/10/2014 11:39:41 AM
Hey guys

I absolutely can't stand the rue tea so I've decided to follow a crystal extraction guide, the Tao of Rue Extraction from this very site to be precise.

I found the filtering process to be particularly difficult but I'm not overly fussed on making the purest, cleanest crystals possible as long as they get the job done so I don't think this has been my problem. I did several filters through an old shirt and the old cotton wool in a funnel trick, but it would have taken longer time than I had available to get all of it through a coffee filter more than once (used several coffee filters and managed to get the whole mixture through once).

Now, I followed the extraction guide, and after having a pile of sodium bicarbonate in the oven for 2 hours at 200c (sitting about 3-4cm deep in a medium sized baking pan) I placed it in my jar with the foul rue tea and I have now had it sitting in my wardrobe for approx. 5 hours. (I am thinking perhaps I should have taken it out several times while it was in the oven and given it a mix around to ensure it all got cooked, you will see why)

While my mixture was still very hot and I had just placed the sodium in I was sure to give it a thorough shake to ensure everything would dissolve but the sodium seemed to just settle right away.

I just checked my mason jar then for the first time since making it and to my great excitement some very small crystals have appeared, however.... There is a layer of sodium carbonate sitting at the bottom of the jar also and it has settled into a hard rock form and that is what the crystals have formed on top of. I will still leave the jar overnight and I'll chuck it in the fridge once my housemate has gone to bed, but I am curious now as to how I will actually get these crystals out. In the Tao guide, the picture shows no sodium sediment at the bottom of the jar after the first round of crystallization but I assume because the pictures in the guide are from a lye mixture instead.

I'm worried that if I was to slowly pour all the liquid out over a filter that I would lose a substantial amount of crystals, and I am worried if I try to break the sodium rock apart in order to scrape the crystals off I will also lose a substantial amount.

The guide does say

After you have decanted the basic (high ph) lye water off the top, you want to add some hot vinegar and water to your freebase alks to redissolve everything back into the solution as harmala acetates. Once your alkaloids are redissolved, filter out anything that won't dissolve. This is mostly plant matter and oils.

So I'm now thinking that tomorrow I should decant as much liquid as possible and then use hot vinegar and water to redissolve the crystals in hopes that the sodium rock also dissolves but that doesn't seem likely to me as it seems to just turn rock solid regardless of water temperature.

Can anybody offer some insight into this? Did I perhaps not cook the sodium right. Like I said it was in the oven for 2 hours at 200c and I even left it inside to be sure, but no guides I read mentioned giving it a mix around so I didn't bother.

Help will be greatly appreciated and sorry about the long read!

Thanks Thumbs up
 
endlessness
#2 Posted : 6/10/2014 12:30:57 PM
You should add the sodium carbonate slowly as you stir the solution to ensure it dissolves well (and that volcano effect doesnt happen while acid is being neutralized by the sodium carb). Alternatively you can also make a saturated sodium carb solution by mixing for example 50ml of water with a spoonfull of sodium carb, shake, then let it decant/filter and add that solution slowly to your harmala solution to precipitate the alkaloids.

Now what you gotta do is with a spoon or something, break the bottom rock a little bit, stir, and let it stand again (maybe some more of the sodium carb will dissolve this way). Then you decant/filter and you redissolve your alkaloids+sodium carbonate excess in acidified water (vinegar), which will indeed neutralizey our sodium carb and make the resulting product (sodium acetate) dissolve in solution. Then you proceed to reprecipitate the alkaloids by adding salt (as in manske precipitation) or by adding a base again (slowly stirring etc)
 
ChaseTheRabbit
#3 Posted : 6/10/2014 12:35:28 PM
endlessness wrote:
You should add the sodium carbonate slowly as you stir the solution to ensure it dissolves well (and that volcano effect doesnt happen while acid is being neutralized by the sodium carb). Alternatively you can also make a saturated sodium carb solution by mixing for example 50ml of water with a spoonfull of sodium carb, shake, then let it decant/filter and add that solution slowly to your harmala solution to precipitate the alkaloids.

Now what you gotta do is with a spoon or something, break the bottom rock a little bit, stir, and let it stand again (maybe some more of the sodium carb will dissolve this way). Then you decant/filter and you redissolve your alkaloids+sodium carbonate excess in acidified water (vinegar), which will indeed neutralizey our sodium carb and make the resulting product (sodium acetate) dissolve in solution. Then you proceed to reprecipitate the alkaloids by adding salt (as in manske precipitation) or by adding a base again (slowly stirring etc)


Great, thank you so much!!!!

Should I use a heated vinegar solution as the instructions say or are you suggesting I just grab a cup or so of straight white vinegar and use that to best dissolve the sodium rock.
 
endlessness
#4 Posted : 6/10/2014 12:41:04 PM
Heat will certainly help it dissolve faster.. And if you are reprecipitating with a manske you should anyways heat to boil and slowly cool down.. If youre gonna just reprecipitate with a base, its not so important but still I think good idea to warm it up a bit to help dissolving.
 
ChaseTheRabbit
#5 Posted : 6/10/2014 1:18:47 PM
endlessness wrote:
Heat will certainly help it dissolve faster.. And if you are reprecipitating with a manske you should anyways heat to boil and slowly cool down.. If youre gonna just reprecipitate with a base, its not so important but still I think good idea to warm it up a bit to help dissolving.


Great - just to confirm I'm heating up a vinegar solution and not straight vinegar right?

And also just a side question for future reference - provided I had done it all right and I didn't have the layer of sodium and just had the desired collection of alkaloid crystals, is it possible to just strain those out, allow them to dry and then consume them as my MAOI (assuming the low levels of sodium carbonate left behind are safe to take?) to save time by not having to do the manske. I'm not too fussed on making the cleanest crystals possible, as long as they do the job I'm happy Smile

Thanks a lot for your help Thumbs up
 
endlessness
#6 Posted : 6/10/2014 2:27:21 PM
yeah heating a vinegar solution but since you have possibly a lot of sodium carb, you might need it to be more concentrated, like instead of just a dash of vinegar, maybe the solution being like 1/4 vinegar 3/4 water.

And yeah you can consume the precipitated alkaloids, just filter/decant . But I do recommend you to redissolve and reprecipitate at least once more, because then dosing will be more accurate.
 
 
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