impatience cost yield(first time)

[GirlsHateMe]

My Unicorn did an extract yesterday, he needed help but my dragon is on house arrest and couldnt come out of his cave.

He did an a/b extract on 40oz of bark, used citric acid, sodium carbonate and some lab grade methylene chloride and naptha to wash the mc.

He had the ph to low for the acid and the ph to high for the base killing his alks. Simply because he was working with to much volume of liquid at one time to really get a feel for how much he was actually adding to the volume. Also he learned later below ph 3 you might be killing some of the alkaloids. And the amount of sodium cabonate he added wasnt quite enough and he added some slowly but still managed to push it up to ph 14 when he was aiming for 12.

He used to much methylene chloride and ended up losing a ton of it trying to decant the majority of the liquid off the top of it due to emulsions that he tried ever so hard to keep away, it hard to swirl liquid with hooves mind you. But he was able to recover about 150-200ml of it. He washed it in warm naptha and stuck it in my freezer. I kept the goo left behind.

He ended up with what looks like a decent amount of pure white crystals that are in my freezer still percip-ing, but its a horrid yield and probably could have been tripled with doing small extracts at a time.

DONT IGNORE THIS! My unicorn swears, small extracts are the way to go after having done a giant one and cussing more than a sailor on shore leave. Which if you've never seen a unicorn get mad and cuss, its so awesome.

Also emulsions SUCK! Hot water running on a mason jar(He has wicked hot tap water) helped so much, saved him a trip to the Griffins cave for rock salt. However I wouldnt be surprised if this also lowered his yield

Anyway just thought id share my unicorns experience since he has a hard time typing with his hooves, just be patient and do small amounts at a time and you will be much happier and your kitchen will be much cleaner.

He doesn't consider this a loss cuz he has something to share with his friends and well from what I hear its awesome stuff in general.

Also, any experience is good experience, he now can do this again with much more knowledge and accuracy. Because no amount of reading is worth a day of experience.

Another peice of advice, when you think youve read everything on here and taken every note you can. Go back and do it again, because chances are youll see some important stuff you missed.

 

[smokeydaze]

Every time seems to present another quiz of problems, until you've gone through them all and can get the job done almost-hassle free.

But can we have some numbers - how much acid did you add to how much water, how many cooks, how much sodium did you add, how many naptha pulls and how much each time, also whats methylene chloride for?

I've heard the ph on both ends of the scale can be pushed out a bit just to play it safe, I doubt much damage was done..

 

[halcyon]

SWIM is curious about the pH issues you mentioned. What reasoning is there that a pH of 2.2 would destroy the already freebase dmt (maxed out pH of citric in water)? Similarly, STB'ers routinely go for pH above and beyond 13 when basifying. SWIM would be amazed if a chemist dropped by and found your range unacceptable. These seem well within the bounds of established practice. SWIM has heard over and over again that emulsions are generally caused by too low of a pH. 69ron is your man here as not many people use a weaker base and DCM.

All help will be read!

{h}

 

[GirlsHateMe]

sorry for the vague story, I diddnt think anybody would really care about numbers but, here they are(glad Brandon st Randy the Unicorn took lab notes now, yes his name is Brandon St. Randy)

He had looked up the mol/l of lemon juice to figure out about how much citric acid to add to the water, which looking back he knows thats retarded because lemons have a ph of 2. Not what he was shooting for, he wanted more of a high 3.
He basicly added about 21-25 grams of acid per gallon. turned the ph paper red in less than a second, not pink, just a hard red.

3 gallons of water for the first boil for about 2 hours, not really a boil at all, just a really heated soak, he never wanted the water to really get a rolling boil on because he was paranoid of heat. Then like a gallon or two for the next two for about an hour each. Again not hard boiling.

He strained the bark and squeezed it till it was pretty dry and did his best to filter out the other gunk but but by then the cheese cloth had seen better times.

I think after all was done he had about 20 liters of water to deal with, and instead of doing the base a little at a time, he found something on here that said 12.5 grams of sodium carbonate per liter of water for a ph of 12, so he adjusted the measurements accordingly and added a bit at a time checking the ph, well when all was added it only came up to about 8-9, so he added more and kept checking it every time and just must have added more than he thought because it managed to get pushed up to 14, maybe higher. But the formula I have here that says the extra sodium carbonate he added would have only pushed it up to about 12.45. So maybe the ph strip wasnt telling brandon the truth or whatever, but im fairly sure he pushed it pretty high and yeah its not a huge deal but he wanted his n-oxide and jungle spice.

Methylene Chloride is basicly DCM, it even says dichloromethane on the bottle. My unicorn knows someone who got ahold of it. Because it holds dmt better than naptha, but also a host of other stuff and he just wanted to be thorough so he grabed some.

Used all 500 ml because like I said, he just used to much being overly thorough. But emulsions formed and while he was decanting alot of it poured out and what he did get he had a tough time getting to separate, but in the end it was done.

Let the mc evaporate for a while till it was dry(couldnt believe how I could watch it dry) and washed it with really warm naptha and stuck the naptha in the freezer and left the goo out to dry.

Ill give more details on the yield after my unicorn drys it out.

But like I said, brandon st randy was just in a hurry and being sloppy, looking back I have no idea why he was in a hurry, he told me something about being over excited and not respecting the process enough.

 

[smokeydaze]

You can be fairly casual about cooking temps, bringing it to a boil then turning it down a little so its just rolling is fine. Also I might of read wrong but you said you had 20L to work with?? Id highly recommend after you filter all the bark out of the mixture to boil the resulting liquid down to around 2-3L. Finally 3-4 pulls of naptha/dcm around 300 ml each time, making sure its reasonably warmed up before putting it in usually get the job done.

 

[GirlsHateMe]

Man randy wanted to boil it down, but he was scared of heat loss and ultimately his paranoia and excitement got the best of him and hindered his extraction.

 

[eindreizig]

You lost a lot when trying to decant?

Then, I take it, you didn't use a separatory funnel. That is pretty key when working with DCM.

You did 40 ounces? That sounds like a lot of water, which when using DCM seems like more of a hinderance.

Next time, may I suggest either using a different solvent (something lighter than water), a giant separatory funnel (3L+), or STB, whatever.

The amount of bark used shouldn't be that much of an issue. For example, a KG is pretty common.

When SWIM uses DCM he uses a soxhlet. There is less liquid.

 

[eindreizig]

Man randy wanted to boil it down, but he was scared of heat loss and ultimately his paranoia and excitement got the best of him and hindered his extraction.

Ayahuasca is boiled in South America to release alkaloids. Also, it is common when using a soxhlet to distill off a large amount of the solvent. Heat shouldn't matter, much.

 

[GirlsHateMe]

You lost a lot when trying to decant?

Then, I take it, you didn't use a separatory funnel. That is pretty key when working with DCM.

You did 40 ounces? That sounds like a lot of water, which when using DCM seems like more of a hinderance.

Next time, may I suggest either using a different solvent (something lighter than water), a giant separatory funnel (3L+), or STB, whatever.

The amount of bark used shouldn't be that much of an issue. For example, a KG is pretty common.

When SWIM uses DCM he uses a soxhlet. There is less liquid.

It was a ton of water, and randy should have reduced it. He thought he could take the water off the top of the dcm easier than it actually was working with so much liquid.

 

[DarkShaman]

He ended up with what looks like a decent amount of pure white crystals that are in my freezer still percip-ing, but its a horrid yield and probably could have been tripled with doing small extracts at a time.

DONT IGNORE THIS! My unicorn swears, small extracts are the way to go after having done a giant one and cussing more than a sailor on shore leave. Which if you've never seen a unicorn get mad and cuss, its so awesome.

Damn. . . . . .what can I say? That really sucks for your unicorn.

I must say, however, that I'm not so sure that small extractions are necessarily the problem. I have performed many extractions using excesses of 200+ grams/mhrb at a time & have yielded quite nicely. However:

Also emulsions SUCK! Hot water running on a mason jar(He has wicked hot tap water) helped so much, saved him a trip to the Griffins cave for rock salt. However I wouldnt be surprised if this also lowered his yield

may explain things a bit. If you are creating emulsions, then chances are that, perhaps, you are a)rushing a simple operation, b)shaking/stirring too vigorously, and/or c)over-analyzing this process, causing sloppiness and unnecessary steps to be taken.

Although. . .

Another peice of advice, when you think youve read everything on here and taken every note you can. Go back and do it again, because chances are youll see some important stuff you missed.

is indeed good advice, experience will eventually bless you with the magic touch of the alchemist. :d


One --> DarkShaman