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Product cleanup advice sought for 69ron cactus limonene tek Options
 
Dipole
#1 Posted : 8/30/2010 5:08:20 PM
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Hi, I'm a new member and this is a long-winded post. The length will, I hope, provide evidence I'm not some nutter and that I consider this fascinating and legitimate research.

I had my first crack at a cactus extraction several weeks back. I used the limonene food-safe tek. I tried to do everything by the book, though I began with fresh San Pedro cactus (not pre-dried powder). Pulled the thorns pulled, sliced off the waxy layer. cored and diced the flesh, and oven dried on as low a setting as I could manage with the oven door open. A portion of the prepared, wet cactus was put through a couple of freeze-thaw cycles before drying.

This reduced about 1.6 kg of wet material and to about 79g of dried. That seems like a low yield, and I may well have over-dried some of it. The dried material was run through a food processor to pulverize into a chunky powder.

After mixing the dried cactus with water, ca. 20g of CaOH, and 250ml of limonene, I hit my first snag. The result was a complete mess of a mixture that could not be separated. It was like wet, green mud and went right through the filter of the French coffee press.

The only way I could think of to get the liquid out was to put the whole mess into a piece of t-shirt fabric and let it drip out (A friend gets the juice out of tiny wild grapes this way). This utterly failed.

I resorted to forcing the liquid out by twisting the fabric and squeezing, a laborious, time-consuming and messy process with a significant loss of liquid into the fabric. (If I’d been using xylene I would have gassed the whole city block.)

I let this first limonene pull settle and it separated into a coloured but clear limonene layer and a cloudy aqueous layer. I separated them with a sep funnel and put the aqueous layer aside. Since the mescaline ought to be in freebase form at this point, I figure the aqueous layer should be mostly unwanted junk. Please challenge my assumption if you think I'm wrong.

The next two limonene pulls went according to plan, with coloured and mostly clear limonene decanted from the cactus mash using the coffee press.

I did three vinegar extracts of each limonene pull, pooled them and evaporated the vinegar using a fan. The result with a thin, tawny brown, waxy, somewhat sticky layer of 415 mg impure mescaline acetate (I presume).


Then I did three carbonated mineral water extracts of each limonene pull, after shaking vigorously in a plastic jug. There was considerable pressure created which distended the sides of the jug, a good sign I believe. Note: I used "designer" bottled water, not just generic soda water, because it had more carbonate or bicarbonate. I now realize all the other dissolved mineral salts might have complicated things.

I pooled the carbonated water extracts and evaporated again using a fan. The result was 4.6 grams of off-white crystalline material scraped from the interior surface of glass baking dish, presumable impure mescaline carbonate (or bicarbonate?)


Finally, the water from the first botched pull was also evaporated using a fan and yielded about 1.5 oz of amber goo of God knows what.


What I’d like is as much pure mescaline as possible, in any salt form, but I’m not really sure what I’ve got or how to clean it?

Bottom line questions: Should I use cold methyl ethyl ketone (MEK) to wash the acetate, and cold 99% (isopropanol) IPA to wash the carbonate, or are there better alternatives? A food safe process would be nice but is not required. And what about the amber goo? Junk, or potential goldmine?

Your advice and comments would be greatly appreciated.

By the way, MEK, as people have pointed out, is trivial to find this in the US in any hardware store. Not so in Canada, but I did find some in a place the specializes in plastics where I guess it’s used to clean up fibreglass resin. Cheap and no questions asked. Also found xylene (unused in this procedure) in a paint store, after much trucking around. Limonene and CaOH I got from the US. PM if you want details.



 

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damon
#2 Posted : 8/30/2010 5:50:10 PM

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Maybe you didn't dry it enough, because it sounds like it was too moist in any case. I always let it sit a day before adding limo, it seems to separate easier. And at that point, I can tell if it will absorb the limo, because it should be pasty and not runny at all. If it is still runny you can just air it out and let it dry. I do it all in a quart mason jar, the limo pours out easy enough, and I use a big spoon to squeeze more out. I don't bother getting it all out, just on the last pull.

Yeah, bad idea with the carbonate water, with the minerals, that's probably mostly what you have. It will be hard to separate from salts without doing a mini a/b. If it was from previously washed limo, I would just use it for a bonus, just take it one day. It probably doesn't contain much. Test it of course. Another thing you could do is just toss it back in with your cactus and pull it back out the regular way. Being dried salts, it shouldn't mess anything up.

For impure acetate, I haven't had much use to clean it up after that. Maybe one day. It already feels much "cleaner" than any resin experience. I do a water recrystallize though. After drying the vinegar, I redissolve in minimal water, leaving behind some lime/calcium and oils that might just be limonene. I filter that into another pan, doing maybe three water washes, until it no longer picks up any tannish color. It is very much like a full spectrum dmt fumarate water re-x.
 
olympus mon
#3 Posted : 8/30/2010 6:24:21 PM

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damon wrote:
I do a water recrystallize though. After drying the vinegar, I redissolve in minimal water, leaving behind some lime/calcium and oils that might just be limonene. I filter that into another pan, doing maybe three water washes, until it no longer picks up any tannish color. It is very much like a full spectrum dmt fumarate water re-x.


could you go into more detail on this step damon? ie/ how much water per acetate, what kind of filter, coffee?, is whats left in the filter waste or actives?
i have 400mg of acetate thats a little gooey and has a strong vinegar smell still. i think i used too much vinegar and it left a lot of residue id like to clean up.
do you think your method would help? w
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damon
#4 Posted : 8/30/2010 8:18:05 PM

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olympus mon wrote:


could you go into more detail on this step damon? ie/ how much water per acetate, what kind of filter, coffee?, is whats left in the filter waste or actives?
i have 400mg of acetate thats a little gooey and has a strong vinegar smell still. i think i used too much vinegar and it left a lot of residue id like to clean up.
do you think your method would help? w


I just use 10ml or so for each water wash, filtered through a funnel with a cotton ball, less water each time. The water will pick up the acetate, and other water solubles, but it would leave the junk behind. You want the stuff that dissolves in water. You don't want anything that does not dissolve in the water. Just remember, the more water you use, the longer it will take to dry, and you will pick up more lime/calcium, so take advantage of the lower solubility of calcium salts. Acetate is extremely bitter, so it is easy to tell if you're leaving any behind.

While it is drying, scrape it up and spread it out with a razor, it dries out faster. It should have a "matte" finish, not glossy. And it should be odorless, not even orangey. Check out the dmt-f water re-x in the wiki, the final drying steps are exactly the same, with a very similar looking result. Or at least mine comes out like that.



 
dg
#5 Posted : 8/30/2010 10:33:02 PM
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doesn't seem like near enough base, but i have little understanding of this tek
what ph did the base get you to?
 
Dipole
#6 Posted : 8/31/2010 4:42:16 AM
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Thanks to everyone for your comments and suggestions, and so quickly!

I may have added too much water to the dried powder. I did let it sit overnight, with stirring from time to time.

When I found I couldn't use the coffee press to squeeze out the limonene on the first pull, I kinda panicked and threw the whole mess into a blender, further homogenizing and liquefying it. Not too clever, because that helped turned it into wet green mud which ran right through the press. Certainly something changed when I got that water out, because the second and third limonene pulls when pretty much by the book.

Re the amounts, the tek calls for 300ml water and 25g of CaOH for 100g of dried cactus, so I just adjusted down accordingly for 79g of cactus to 225ml water (Actually not water but the liquid that leaked out of the cactus that had been through the freeze-that cycles. Rather than evaporate it with the drying cactus, I used it instead of water to rehydrate the dried cactus into paste. Another little innovation that might not have been so clever.

Don't see any notes about what the pH was, though I did measure it with pH paper and I thought it was sufficiently alkaline.

I suppose the carbonate extraction might be a dog's breakfast of various mescaline salts and inorganic salts. But even if the mescaline is in a variety of salt forms, that just makes dose problematic.. They should all be active, no?

Also, could not some particular "magic" acid (let's say hydrochloric) be used to displace all the anions like carbonate, sulphate, nitrate and whatever else and leave just mescaline hydrochloride which might be more easily cleaned up. I'm out of my league here.

I could try a water wash of the acetate, but I've got so little of it! I could also just evaporate a bottle of designer mineral water and see what's left, as a comparison. Or, just gingerly test the impure carbonate. At least the colour isn't alarming.

Anyone have any idea what the amber goo is. It's been in the fridge for weeks and is almost solid, or at least a very, very viscous liquid. Isn't it likely it's just water soluble trash?
 
 
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