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D-limonene extraction guide for first timer - safest possible method Options
 
iamalien
#1 Posted : 3/16/2022 3:25:06 PM
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Hi

Thanks to everyone who allowed me to be a full member and post here, much appreciated. Great community.

I am trying to follow best practice and harm reduction, not concerned with price or losing some efficiency. I am unable to setup a Separating Funnel however so plan to do that part with pipettes and safety gear.

I will be using the following guide but creating a more detailed accurate version and potentially deviating at the end, it is a work in progress:

https://psychonautwiki.o...ctrum%22_DMT_extraction

I will also be trying to use the best materials and equipment possible.

I have come up with the following list to start with and would really appreciate some feedback from the experts:

Erlenmeyer with glass stopper (using d-limo to stop the stopper sticking -ok?)

Pipettes

Glass rods

Glass Beakers

lye
Debating sodium carbonate as safer but I heard lye is better and as long as wear gloves and mask should be ok. I would like to hear others experiences though please.

d-limonene - anyone know of a good UK source please? Still looking.
Food grade 100% and not imported.

Storage for d-limonene after use - what is best for this? Concern over the metal top reacting if I use glass jar.

This just leaves safety equipment and finalizing the process: goggles, mask, gloves, suit? plus scales, PH tester and temp gun which I will leave for another post.

Thanks in advance
 

Live plants. Sustainable, ethically sourced, native American owned.
 
iamalien
#2 Posted : 3/16/2022 3:59:44 PM
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for d-limonene this is the best I can find so far without importing or buying off random sellers on ebay

https://apcpure.com/prod...tribute_pack-size=500ml

https://pellwall.com/sho...olates/orange-terpenes/

but I cannot see what the 4-6% is.

I think I found a winner here

https://www.terpenes-uk....k/product-page/limonene

https://23d34d56-8a16-43...89b94c22afdf73ac1d6.pdf

3. COMPOSITION/INFORMATION ON INGREDIENTS
Chemical name - CARVENE

Common name and synonyms -
DIPENTENE
(+)-P-MENTHA-1,8-DIENE
(R)-(+)-Limonene
(R)-4-Isopropenyl-1-methyl-1-cyclohexene
1- methyl-4-prop-1-en-2-ylcyclohexene

CAS number - 5989-27-5

100%
 
shroombee
#3 Posted : 3/16/2022 5:00:17 PM

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The Q21Q21 TEK (lime, limonene, vinegar) has more detail than the one posted on Psychonaut Wiki:

https://wiki.dmt-nexus.m...Lime_A/B_Extraction_Tek

Using DMT acetate for oral pharma is fine. However, check this regarding concerns about smoking acetates. If you look around, there are some other threads that raise the same concern:

https://www.dmt-nexus.me...spx?g=posts&t=66118
 
iamalien
#4 Posted : 3/16/2022 5:14:15 PM
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Hey thanks for the feedback I had forgotten about that guide, will reread.

I was discussing acetate conversion with Homo Tryp. and they mentioned there were various ways to convert this to freebase, like using fumaric acid. This is one thing I wanted to discuss, to find the best method.
 
Homo Trypens
#5 Posted : 3/16/2022 7:29:09 PM

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iamalien wrote:
Hey thanks for the feedback I had forgotten about that guide, will reread.

I was discussing acetate conversion with Homo Tryp. and they mentioned there were various ways to convert this to freebase, like using fumaric acid. This is one thing I wanted to discuss, to find the best method.


Fumaric acid is an alternative to acetic acid for the backsalt. It leads to fumarate instead of acetate, both are salt forms. Acetate is usually a goo, whereas fumarate is a solid.

Both acetate and fumarate can be converted to freebase. Freebase from acetate often stayed oily for me, from fumarate i didn't have that problem.
3 fumarate to freebase conversion teks
#3 also works with acetate. I haven't tried #1 and #2 with acetate.


The Backsalt:

With fumaric, you have the option to do FASA or FASI (Fumaric Acid Saturated Acetone or Isopropanol). You just
- mix the FASA/I with the dmt-containing d-limonene,
- the fumarate crashes out and can be
- collected in a coffee filter
- (and washed with cold ipa/acetone to remove most of the orange smell).
This yields pretty clean product ime.
Only downside, your d-limonene then has to be washed several times to remove the acetone or ipa before you can reuse the limo. The acetone or ipa is lost unless you're ready to distill.

I don't know of any way to replicate this with acetic. I simply
- used 5% acetic in water to liquid-liquid extract from the d-limonene,
- separated the bottom aqueous layer from the upper limo layer,
- repeated the previous steps 3x,
- combined and evaporated the water.
This can of course be done with fumaric too, it's called FASW then.
You should be careful with the temperature towards the end of evaporating the water! Acetate is burnt easily.
With this method, you can reuse the d-limonene without cleaning it if you want.

---
edit / add on:

Note that you should pull from your soup with d-limonene at least 2, probably 3 times.

With the water based method, you can reuse the same limo after each backsalt for the next pull.

With FASA/I, you might want to use 'fresh' limo for each pull, combine the pulls and do the backsalt just once.
Or backsalt each pull separately (to see which pull yielded how much), but combine the acetone/ipa contaminated limo for the washing.
 
Homo Trypens
#6 Posted : 3/16/2022 7:30:13 PM

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iamalien wrote:

...

I think I found a winner here

https://www.terpenes-uk....k/product-page/limonene

https://23d34d56-8a16-43...89b94c22afdf73ac1d6.pdf

3. COMPOSITION/INFORMATION ON INGREDIENTS
Chemical name - CARVENE

Common name and synonyms -
DIPENTENE
(+)-P-MENTHA-1,8-DIENE
(R)-(+)-Limonene
(R)-4-Isopropenyl-1-methyl-1-cyclohexene
1- methyl-4-prop-1-en-2-ylcyclohexene

CAS number - 5989-27-5

100%


Looks like you did Smile
 
iamalien
#7 Posted : 3/17/2022 10:26:21 AM
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Thanks for the feedback - really appreciated.

So looking at both teks the difference is I am adding vinegar at the end not the start as with Q21Q21. Homo Trypens did you suggest adding water at the start and using vinegar at the end to "salt" it out and most likely moving on to fumaric acid after that as it results in a better end product?

Either way I plan to turn it to freebase using sodium carbonate and then dissolve in ethanol and add to leaf to make changa which should solve the issues with smoking acetate.

The other differences are Q21Q21 uses lime but I was told this is not the best to work with (one being it prefers drier mixtures) and to use either lye or sodium carbonate. I would prefer sodium carbonate but does it create too much emulsions? and is it way less efficient? Otherwise could work...

 
Homo Trypens
#8 Posted : 3/17/2022 6:01:27 PM

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iamalien wrote:
...

So looking at both teks the difference is I am adding vinegar at the end not the start as with Q21Q21. Homo Trypens did you suggest adding water at the start and using vinegar at the end to "salt" it out and most likely moving on to fumaric acid after that as it results in a better end product?

...


You can add a bit of acid for the boiling, it helps the dmt migrate into the water. This can be pretty much any acid - vinegar, citric, ... And it doesn't take very much. Just get your pH below 4. If you soak MHRB in distilled water for long enough, pH will eventually drop to that range by itself due to the tannic acid from the bark. So acid addition for this stage is not strictly necessary but recommended. You do need water though.

I was talking about the backsalting, which you do after
- you based the soup,
- pulled the freebase with d-limonene and
- cleanly separated the d-limonene from the soup.
You do not add acid to the soup after it was based.

You use acid to convert the dmt into a salt, so you can get it out of the d-limonene. It's not acetic then fumaric though, it's one or the other.
If you wanna do water based backsalt and evap, you can choose freely.
If you wanna precipitate salt directly, you need fumaric and either acetone or isopropanol.

In my extractions, i have achieved purer results with FASA than with water.
 
Loveall
#9 Posted : 4/2/2022 11:14:38 PM

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One can use benzoic acid granules directly to salt the limonene. Benzoic acid is used in the food industry and is easy to find, at least in my country. The process is experimental but seems to work. No need to fuss with separate FASI. I believe FASA is problematic as fumaric acid will crash from FASA in limonene if I recall correctly.

Benzoic acid salted limonene can be reused without washing, any excess acid reacts with the lie in the bark and is removed during extraction (wash and extract in one step).

A drying agent is a good idea to remove cloudiness from micro emulsions before salting.

Just an experimental option if anyone is interested.

Edit: Here is a discussion regarding FASA/limonene
 
 
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