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I have a question for 69ron's d-limonene extraction...i am so confused and need help :( Options
 
Doctor_dick
#1 Posted : 12/8/2009 5:53:24 PM
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okay....here is my problem...fallowed the tek exactly as said...so first scraping/yield comes out exactly as 69ron said it would, waxy, amber colored stuff...not very powdery whatsoever, and i got a very nice yield like he said i would....unfortunately i didnt take a picture of the pryex dish before i scraped it, but i did take a picture of the acetate after i capped it all up...heres the first pull all capped



after that, went through the steps again exactly the same, but this time on my next pull, after drying all i got was a very small amount of opium type goo....i was confused i thought my cactus was already spent but i was like this cant be...so i guess my first question is why in the world did it come out as a small amount of brown goo and not the waxy acetate i was suposed to get?

so i decided to have another go...so i put a couple extra grams of sodium hydroxide in the mix cus i thought that was the reason it didnt crystalize on the dish this time around.

on my third pull, well second pull really because the other "second" pull gave me nothing. so on this next pull, this is what i got. this really confused me




this confused the crap out of me...nothing even remotely waxy or amber...a slightly off white and very dry powder! this is the most confusing part and where all my questions are. could it be becaue i added like 2 or 3 extra grams of sodium hydroxide to the mix? how could i have such a drastic change in my final product and why does it look like this? has anyone seen acetate look like this? is this gonna be active and have a fair amount of mescaline in it in similar quantaties as the waxy slightly brown stuff? i will eventually test it out but it may not be for a while...

well, so i decided to do one final pull....i ended up with a brown product this time, but still very dry powder andnot the waxy stuff i was expecting to get...

so i hope you guys can answer this. i'm really puzzled.
 

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damiana
#2 Posted : 12/8/2009 7:14:54 PM

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Okay, for the second pull, if you didn't let the d-limo sit in the cactus again but went right to the second pull, well you wouldn't get as much. If you did let it sit, and stirred it, then did the second pull, well this could be that maybe the d-limo wasn't getting any alkaloids cause the cactus wasn't basified enough. So you based it again with lots of sodium hydroxide and got that off white powder. A few questions, for every pull did you heat the vinegar or let it evap. at room temp? Also where did you get the cactus from?
PEACE
 
Doctor_dick
#3 Posted : 12/8/2009 7:41:28 PM
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damiana wrote:
Okay, for the second pull, if you didn't let the d-limo sit in the cactus again but went right to the second pull, well you wouldn't get as much. If you did let it sit, and stirred it, then did the second pull, well this could be that maybe the d-limo wasn't getting any alkaloids cause the cactus wasn't basified enough. So you based it again with lots of sodium hydroxide and got that off white powder. A few questions, for every pull did you heat the vinegar or let it evap. at room temp? Also where did you get the cactus from?


i heated it but not alot of heat...150 in the oven

i stirred every time which is why im confused and let it sit every time

i got the cactus from heavenly products (are sources allowed?) it was dried torch flesh i powdered my self (seems pretty potent)
 
damiana
#4 Posted : 12/8/2009 7:49:39 PM

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Sources are allowed, we talk about them often. Yeah heavenly products is good stuff. The off white powder could well be un-active sodium hydroxide, not sure (I'm no chemist), but you might want to test it. The first pull looks good! Smile The last brown pull is probably active as well as the second. I'd keep pulling, I always got more when I pulled up to 6 or more times. Someone else might enlighten this situation, though I wouldn't worry for now, have fun.
PEACE
 
Virola78
#5 Posted : 12/8/2009 10:50:27 PM

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is the powder alkaline or acid?
you can probably test with some pH paper and a drop of water..
“The most important thing in illness is never to lose heart.” -Nikolai Lenin

I know that you believe you understand what you think I said, but I'm not sure you realize that what you heard is not what I meant.
 
elphologist1
#6 Posted : 12/9/2009 1:12:34 AM
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Virola78 wrote:
is the powder alkaline or acid?
you can probably test with some pH paper and a drop of water..


Yeah test if it is basic - if so you probably have contamination with sodium hydroxide. Another way to tell is leave it in a humid environment and check if it becomes wet - sodium hydroxide does. And finally, sodium hydroxide absorbs carbon dioxide from the air making sodium carbonate. Take a small amount of the powder (after it has sat out in the air for a while) and add an acid such as vinegar or dilute hydrochloric acid. If it fizzes, you have sodium hydroxide/carbonate besides your desired product.

elphologist

 
Infundibulum
#7 Posted : 12/9/2009 4:50:08 AM

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elphologist1 wrote:
Virola78 wrote:
is the powder alkaline or acid?
you can probably test with some pH paper and a drop of water..


Yeah test if it is basic - if so you probably have contamination with sodium hydroxide. Another way to tell is leave it in a humid environment and check if it becomes wet - sodium hydroxide does. And finally, sodium hydroxide absorbs carbon dioxide from the air making sodium carbonate. Take a small amount of the powder (after it has sat out in the air for a while) and add an acid such as vinegar or dilute hydrochloric acid. If it fizzes, you have sodium hydroxide/carbonate besides your desired product.

elphologist


What kind of rubbish are you guys talking about here?!?!?!

Doctor_dick, you're doing fine here, no problem. Try testing with your tongue or smell the product if you're unsure. Try testing the results from the first pull with the ones from the 3rd one

Others please note that he used calcium hydroxide, not sodium hydroxide. Also note that if there ever was some base contamination it would have reacted and get neutralised by the vinegar back0salting step to give calcium acetate (or sodium acetate). I don't even want to think the OP trying all those useless advices you gave him!

Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
Touche Guevara
#8 Posted : 12/9/2009 5:41:09 AM
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The OP says NaOH, Infundibulum.
 
Infundibulum
#9 Posted : 12/9/2009 12:00:15 PM

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Touche Guevara wrote:
The OP says NaOH, Infundibulum.

Yeah, but he also says that he "...followed the tek exactly as said...". This is a mescaline extraction tek and it is 69ron's non-toxic calcium hydroxide/limonene/vinegar tek. It is likely however that even if the OP didn't mean "sodium hydroxide" when he wrote "...so i put a couple extra grams of sodium hydroxide..." he may have added few grams of it in the Ca(OH)2/limo/cactus mix.

The fact that no base can be present in the final product after the vinegar evaporation does not change however, thus making the advice of elphologist1 unnecessarily complicated and blatantly misleading. In the worst case the OP may have the presence of calcium acetate or sodium acetate. No sodium hydroxide or calcium hydroxide.


Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
Virola78
#10 Posted : 12/9/2009 12:52:57 PM

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Infundibulum wrote:
elphologist1 wrote:
Virola78 wrote:
is the powder alkaline or acid?
you can probably test with some pH paper and a drop of water..


Yeah test if it is basic - if so you probably have contamination with sodium hydroxide. Another way to tell is leave it in a humid environment and check if it becomes wet - sodium hydroxide does. And finally, sodium hydroxide absorbs carbon dioxide from the air making sodium carbonate. Take a small amount of the powder (after it has sat out in the air for a while) and add an acid such as vinegar or dilute hydrochloric acid. If it fizzes, you have sodium hydroxide/carbonate besides your desired product.

elphologist


What kind of rubbish are you guys talking about here?!?!?!

Doctor_dick, you're doing fine here, no problem. Try testing with your tongue or smell the product if you're unsure. Try testing the results from the first pull with the ones from the 3rd one

Others please note that he used calcium hydroxide, not sodium hydroxide. Also note that if there ever was some base contamination it would have reacted and get neutralised by the vinegar back0salting step to give calcium acetate (or sodium acetate). I don't even want to think the OP trying all those useless advices you gave him!



Yea it was already clear to me he used NaOH instead of CaOH. If he used way too much NaOH (and it somehow got into the vinegar, maybe because it did not dissolve in the cactus-water-base-limo-mix and was in this way (through the emulsion) carried over to the vinegar) then he would have more then neutralised the vinegar I figured. Remember there is only small volume of vinegar used in the limo tek). Then there could be some bases present in the endproduct. Yes, next to Na-acetate that is, duh!

Not THAT far fetched... Was just trying to offer some first aid. Im just like you waiting for the experts to have a look at this. No need to get all excited about it. And still, whatever happened (I was not there, and the tek was obviously NOT precisely followed), if it were my stuff, I would surely want to know if there are any sharp bases in there. I would not take any risk consuming basic salts.

My advise was easy and innocent (following my advise would not cause any new problems whatsoever).

So pls...




“The most important thing in illness is never to lose heart.” -Nikolai Lenin

I know that you believe you understand what you think I said, but I'm not sure you realize that what you heard is not what I meant.
 
Infundibulum
#11 Posted : 12/9/2009 1:21:05 PM

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Of course mate, there's no problem!

Any advice is usually more than welcome but some of them can be waaay off! Hence the intervention


Virola78 wrote:
Remember there is only small volume of vinegar used in the limo tek). Then there could be some bases present in the endproduct. Yes, next to Na-acetate that is, duh!

Not THAT far fetched...

Wrong. 5% vinegar is a lot of vinegar and would have normally neutralised every base traces. For instance, 50ml of 5% vinegar can fully neutralise 1.6g of NaOH or 1.5 grams of Ca(OH)2. Do you hence imply that there was such a carryover of base in the emulsion that all the vinegar could not neutralise it?


Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
soulfood
#12 Posted : 12/9/2009 1:42:05 PM

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I can more than verify infundibulum's statement, what with NaOH being insoluble in limonene you'd definately be dealing with only trace amounts that would barely alter the pH of the vinegar solution if at all, same as when salting out DMT from a high pH STB.
 
Virola78
#13 Posted : 12/9/2009 2:00:44 PM

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Indeed no problem m8 : )
How could there be? Im in love with all of you...

And I very much like the fact that this guy is helped by you. Very reassuring because some monkey will be doing this experiment soon.
So I am very very interested in the outcome of (solution to) this problem.
Eager to learn, eager to try...


“The most important thing in illness is never to lose heart.” -Nikolai Lenin

I know that you believe you understand what you think I said, but I'm not sure you realize that what you heard is not what I meant.
 
Doctor_dick
#14 Posted : 12/10/2009 4:24:22 AM
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feeling foolish, i definitely meant calcium hydroxide...Embarrased

I think I will try doing 69rons mesc HCL tek next time instead...i know i can get bigger yields/stronger product w/ acetate, but i can't help but love perfect white fluffy powder that is consistently coming out the same every time Cool aesthetics is imprtant to me somewhat...

luckily I still have 600 grams of torch left and have alot of calcium hydroxide on the way...need to order some more limonene though...i just love doing extractions man so much fun! will be even better when i have my sep funnel all set too Smile
 
antichode
#15 Posted : 1/11/2010 8:52:13 AM

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That third pic definitely looks fishy. Thats what Mescaline HCL looks like after its been washed with Acetone! There's no way that was pulled straight from limo with vinegar like that

Despite the reasoning in this thread Id be inclined to think that is Calcium Hydroxide. Although what Infundibulum says makes sense SWIM has personally seen more than a few grams of Ca(OH) be squeezed out of the mix along with limonene. SWIM squeezes his cactus through a t-shirt, and if you squeeze too hard grey water comes out that is chocka full of Ca(OH). SWIMS Ca(OH) is super super fine and it passes through filters along with the water

Doctor_dick wrote:
i can't help but love perfect white fluffy powder that is consistently coming out the same every time Cool


The HCL tek is pretty much exactly the same, just a bit more fidly in terms of mixing the desired strength of acid.

SWIMS HCL extractions yield a sticky black tar with no crystal formations to speak of. Its sticky as hell and absorbs moisture quickly. However.... Once the tar is mixed in a jar with acetone the mixture clouds up and off white mescaline falls to the bottom in no time, its very easy to clean thoroughly in this manner


 
ThirdEyeVision
#16 Posted : 1/11/2010 5:57:58 PM

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A friend of mine uses a French press in this tek and squeezes out the Limo so does in fact get some carry over of calcium hydroxide. He had a contamination that looked almost exactly like this. He washed with acetone and problem was solved. I can post before and after pics if needed.

What I'm wondering about though, was there a MEK wash done on the first pull (the one in capsules)? There must have been, because my friends never looked like that straight from the vinigar.
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