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Rayman74
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69Rons D-Limonene extraction fail.
#26976293 - 10/08/20 11:35 PM (3 years, 3 months ago) |
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Hello
Was up for my first attempt at extracting mescaline so I thought I'd give 69Ron's Limonene extraction a go as the proceedure seemed simple enough, the reactants easy to aquire ( although cacti & limonene expensive ), and the relative non toxicity of the reactants used.
I've also done enough stupid regrettable things in my life to know that creating products with serious acids and bases might not end well with my lack of experience in the field of chemistry. So essentially I didn't want to do anything that would add yet another unforgettable moment into the ledger of shame.
So starting with 5 very decent sized mature cuts each about 1ft in length I despined, and deskinned ( the waxy cuticle ) and de-cored each section.
( Its worth noting here that if you ever intend to peel away the waxy cuticle on mature San Pedro make sure you dont use your finger nails to do so. The cuts you can easily get under your fingernails from the waxy cuticle edge hurt like a mofo. After learning that lesson I used a blunt butter knife which made the whole process a lot easier as well. )
So with all the desired cacti de-cored and deskinned I cut the pieces into thumb sized chunks and put in ziplock bags into the freezer to freeze then rethaw three times over to lyse the celluar matter as much as possible.
Once that was done I dehydrated the slimey cacti contents in a food dehydrator set to 65degC.
After 14 hours the pieces were dried nicely with a candy like feel and snapped when folded.
I was tempted to just eat it like that as the smell wasn't all that off putting and amongst the bitterness of the alkaloids there was an almost caramalised quality to it.
But the memories. Last time I tried to down a pint of boiled SP ( Boiled and reduced with lemon juice for many hours ) it didn't go down for long and I projectile vomited over the balcony, the contents largely settling onto my housemates hanging plant. It was a succulent so it did survive that onslaught but she did complain of the smell of vomit when she watered the plant days later.
So extraction it was going to be.
After weighing the dried cactus the total amount came up to 70 grams.
So step 1 of the process was to grind 100grams of the dried cactus into a fine powder and mix with 25grams of food grade calcium hydroxide and mix in 300ml of water for 5 minutes.
I have heard that the fine particles of ground cacti can be a pretty nasty irritant if inhaled or if it gets into your eyes so I did use a mask and goggles for this process. So using PPE and armed with a coffee grinder I powdered it till it was fine powder taking great care not to inhale the smoke like cacti aerosols that were disperesed each time when opening up the grinder to get the contents I even waited a good minute before removing the lid after each grind but the fine misty powder has some serious hang time to it.
Now a decision to make. As I only have 70grams of cacti do I ratio down the CaOH and H2O to match or do I keep those and everything else in the proceedure as they are and just use less cacti.
I opted to leave the CaOH at 25g and water at 300mL thinking that as long as those two are balanced then a little less of the cacti wouldn't matter all that much? This could have been where I went wrong?
The consistency was what I expected. Not too wet. Kind of like concrete paste with high workability. Looked like grey green grainy cottage cheese with no water pooling anywhere. At this point I figured things seemed to be going pretty well. There was clearly a chemical reaction happening as there was some bubbling and heat generated when stirring which I did for a period of somewhere between 5 and 7 minutes. I thought that perhaps I should leave it for longer before adding the limonene as the added time might assist with bringing more alkaloids out of the cacti. But then I ultimately don't know what the repurcussions might be for leaving it too long in the strong base paste so I decide to stick to the tek as written even though 5 odd minutes really isn't a very long period of time. This also could have been where I went wrong?
So adding the limonene ( 300mL of ) to the paste I mix it in thoroughly and I leave it for the 3 hours required in step 2. Every now and then I can't help myself with periodic visits to stir it like an enthusiastic wizard.
When 3 hours is up I pour everything into a french press and pour the oily limonene through a Harris number 4 paper coffee filter. I probably go through about 4 filters until all the oil is pressed and passed through the filter. This is another point where I could have gone wrong? Do coffee filters vary in their pore size enough that the alkaloids desired could be filtered out completely by a poor choice of filter?
So I then put the limonene into the sep funnel and add 25ml of vinegar ( Cornwalls White Vinegar ) and gently roll and tumble and agitate the vinegar through the limonene for a few minutes with some light shaking. I dont shake vigerously as I have heard that you can end up with an emulsion that can take a long time to settle out again. The vinegar still apperas to be largely clear at this point. Is this where I went wrong. Was I supposed to be a lot more vigorous with the shaking here? Or should I have left the vinegar in contact with the limonene for much longer than a few minutes?
Once I drained the vinegar out of the sep funnel I once again added the vinegar back into the sep funnel two more times and did two more pulls from that batch of limonene. I then return that limonene to the cacti base paste created before and add more limonene to make up the shortfall to get 300mL of limonene again.
When repeating the whole thing again for the second time the tek says repeat steps 2 through 6 at least twice. I don't rebasify the paste by adding new CaOH or H2O again as that doesn't seem to be implied in the tek as that is step one right?
So I leave the limonene in the reused paste overnight and then do everything again the following day. When I do it the second time around the D-Limonene is quite cloudy and opaque after its long sit in the cacti paste.
Now when I put the pyrex out to evaporate the vinegar it hits me. I've fucked this up. Why is that solution so damn clear. If its loaded with alkaloids that are going to present themselves as a waxy amber residue after evaporation then surely that vinegar solution I am looking at should be opaque oui.
The solution does have a slight straw tint visible in the pyrex but I'm pretty sure the whole thing is all over now.
So once again.
Was it :
1) Wrong ratios dude. You actually fucked up step one you dildo. 2) Yer didn't basify it long enough ya plonker. ( I almost suspect this but I don't know ) 3) You used what kind of coffee filter? What were you thinking man. We all skip that step. Just dont get the green shit into the sep funel when pouring the limonene into it you donkey. ( Of course I know a coffee filter is used here but can they filter too much if not the right grade? ) 4) You're supposed to shake it till that shit turns cloudy. No it doesn't say that in the instructions but isn't it obvious you fool.
or perhaps it is 5) Your cactus has no alkaloids in it maaaan. I don't buy the last hypothesis at all as there should have been some opacity in the vinegar whether the cactus had some chutzpah or not.
Any suggestions as I am foolish enough to do this all over again whenever I can source SP somewhere that isn't 100 bucks a metre.
( No I didn't pay that much. I'm not that much of a donkey. )
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hummingbird

Registered: 06/29/14
Posts: 2,134
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Re: 69Rons D-Limonene extraction fail. [Re: Rayman74]
#26976308 - 10/08/20 11:49 PM (3 years, 3 months ago) |
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Did you evaporate all the vinegar...was there nothing on the dish?
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Rayman74
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Registered: 10/08/20
Posts: 6
Loc: Australia
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Re: 69Rons D-Limonene extraction fail. [Re: hummingbird]
#26976311 - 10/08/20 11:53 PM (3 years, 3 months ago) |
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It's still evaporating now.
The vinegar should be cloudy if tek is done correctly though right?
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hummingbird

Registered: 06/29/14
Posts: 2,134
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Re: 69Rons D-Limonene extraction fail. [Re: Rayman74]
#26976322 - 10/09/20 12:07 AM (3 years, 3 months ago) |
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I can't remember if it was cloudy when I did it honestly, probably doesn't need to be though. When all the vinegar evaporates you will know for sure if it worked.
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Northerner
splelling chceker


Registered: 07/29/12
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Re: 69Rons D-Limonene extraction fail. [Re: hummingbird]
#26976411 - 10/09/20 03:31 AM (3 years, 3 months ago) |
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Whatever you decide to do, don't throw out your plant matter/basic soup until you have your prize.
Alkaloids don't evaporate. If they are there you just have to figure how to get them out.
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The nearest we ever come to knowing truth is when we are witness to paradox.
Edited by Northerner (10/09/20 03:46 AM)
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Rayman74
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Loc: Australia
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Re: 69Rons D-Limonene extraction fail. [Re: Northerner]
#26976448 - 10/09/20 04:56 AM (3 years, 3 months ago) |
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Ummm yes.......About that.
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Northerner
splelling chceker


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Re: 69Rons D-Limonene extraction fail. [Re: Rayman74]
#26977200 - 10/09/20 03:26 PM (3 years, 3 months ago) |
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Rookie mistake, almost all of us do at least once it unless warned. You can always do multiple extractions on the same material and continue to get (diminishing) results.
Do you see anything more now it's evapped down a bit?
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The nearest we ever come to knowing truth is when we are witness to paradox.
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Rayman74
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Loc: Australia
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Re: 69Rons D-Limonene extraction fail. [Re: Northerner]
#26977587 - 10/09/20 08:21 PM (3 years, 3 months ago) |
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Yes.
hummingbird seems to be correct.
The vinegar solution is becoming a darker gold tint as it evaporates.
May yet get at least one experience out of it which would be great as I am at a point in my life where I could really use the insight.
Will know for sure whether there are any reasonable solutes left over about 24 hours from now.
Unfortunately I went through two cheap food dehydrators with this experiment so am now evaporating solution using gentle wind and sunlight. Next time I buy a dehydrator I will definately go with a quality brand.
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Northerner
splelling chceker


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Posts: 14,141
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Re: 69Rons D-Limonene extraction fail. [Re: Rayman74]
#26977760 - 10/09/20 11:16 PM (3 years, 3 months ago) |
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Hope your extraction works out. 
Lash out on a good dehydrator. A good dehydrator pays for itself in no time. Cactus, mushrooms, jerky, fruits, you name it.
Last time I was lucky to get a really good one second hand barely used, maybe 10 years ago. Made in New Zealand of all places. Didn't know those guys made anything non-agricultural.
ps: where are you? I'm up far North QLD.
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The nearest we ever come to knowing truth is when we are witness to paradox.
Edited by Northerner (10/09/20 11:29 PM)
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Rayman74
Stranger
Registered: 10/08/20
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Re: 69Rons D-Limonene extraction fail. [Re: Northerner]
#26977832 - 10/10/20 01:08 AM (3 years, 3 months ago) |
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I'm from the big city in the state below yours.
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Northerner
splelling chceker


Registered: 07/29/12
Posts: 14,141
Loc: FNQ
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Re: 69Rons D-Limonene extraction fail. [Re: Rayman74]
#26977838 - 10/10/20 01:17 AM (3 years, 3 months ago) |
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Hope you're dealing with the whole covid fuckup okay man. The border's are mostly open now anyways.
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The nearest we ever come to knowing truth is when we are witness to paradox.
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hummingbird

Registered: 06/29/14
Posts: 2,134
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Re: 69Rons D-Limonene extraction fail. [Re: Northerner]
#26977906 - 10/10/20 03:18 AM (3 years, 3 months ago) |
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Cool, I hope you are pleasantly surprised when it all evaporates. Most of the time alkaloids won't cloud solutions unless it's pretty saturated and/or cold IME.
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Typerwritermonky
shboop a doop a doop


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Re: 69Rons D-Limonene extraction fail. [Re: hummingbird]
#26979162 - 10/10/20 09:50 PM (3 years, 3 months ago) |
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Good luck, lots of people have a lot of trouble with rons d-limonene teqs so dont sweat it. Some folks swear by it, others say it never works weven when followed perfectly.
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Marmie
Peter peter portion eater



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Typerwritermonky
shboop a doop a doop


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Re: 69Rons D-Limonene extraction fail. [Re: Marmie]
#26980186 - 10/11/20 03:26 PM (3 years, 3 months ago) |
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I mean if you read through that shroomdoom tek you can see NOBODY can get it right and almost a half dozen folks tried who are noted quality home chemists and failed to replicate it and got NOTHING.
Maybe try the Ekstaza's tek. Otherwise, fuck the d-limo and use stb then xylene/toulene.
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SpacedX
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Re: 69Rons D-Limonene extraction fail. [Re: Northerner]
#26994820 - 10/20/20 03:33 PM (3 years, 3 months ago) |
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Quote:
Northerner said: Hope your extraction works out. 
Lash out on a good dehydrator. A good dehydrator pays for itself in no time. Cactus, mushrooms, jerky, fruits, you name it.
Last time I was lucky to get a really good one second hand barely used, maybe 10 years ago. Made in New Zealand of all places. Didn't know those guys made anything non-agricultural.
ps: where are you? I'm up far North QLD.
We don't. It's all milk powder and lamb chops. Are you sure it's not a NZ brand thats made in China?
I brought a separate dehydrator for the cactus as I didn't feel right drying the kids apples out in the same one.
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SpacedX
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Re: 69Rons D-Limonene extraction fail. [Re: SpacedX]
#26994826 - 10/20/20 03:35 PM (3 years, 3 months ago) |
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Hey OP. I don't think you should assume failure until the evap has finished.
Two tips. You should leave the vinegar in the orange oil for hours not min. Swirl it gently every once and a while, leave it overnight.
You should also use fresh vinegar each time you do a vinegar pull.
If all else fails then try a stronger acid like the HCL mentioned in the tek. All the rest of your steps look fine.
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Rayman74
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Re: 69Rons D-Limonene extraction fail. [Re: SpacedX]
#27000729 - 10/24/20 01:39 AM (3 years, 3 months ago) |
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Hello SpacedX
Yeah it wasn't a complete failure.
Only managed to get about 100mg of amber residue in the end.
Consumed it for mild effect. A little like an LSD trip that didn't quite take hold. No visuals but perception was very much altered for many hours. Woke up feeling very cloudy headed the following day.
In the end I did come to the same conclusion SpacedX in that I probably went wrong in not leaving the vinegar in the orange oil for anywhere near long enough.
As you suggested I did use fresh vinegar for each pull. Upon rereading my OP days later I did notice that had made a mistake where I should have said "once again added 25mL more vinegar back into the sep funnel two more times" as opposed to "once again added the vinegar back into the sep funnel two more times"
Very sloppy and confusing on my part.
Anyhow I'm glad that someone has confirmed my suspicions on that theory so thank you for your post and overall analysis. It's good to know that hours as opposed to minutes for the alkaloid transfer into vinegar is the more likely way to achieve success here.
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