Basic Extraction Process Questions??

[JohnIce2]

If this is already part of a thread I'm sorry: due to not being a full member their are alot of places on the Nexus that I cannot post.

So in theory would the below process work for ACRB or Chali.?

1: Take plant material and soak in 10% Acetic Acid while stirring/ shaking for about a hour on and off.
Let solution sit for 3 more hours shaking here and their.

2: Defat with Naphtha (Is this Petroleum Ether?) by pouring small amounts into solution, stirring, then siphoning off to waste jar (Repeat a few times depending on which plant is used and its fat content).

3: Take 70% IPA and mix into solution pouring the same amount (ml) of vinegar used previously, then add non iodized table salt and mix until the layers separate. (Will the alcohol take in your alkaloids? Are they more soluble in alcohol as compared to vinegar water?)

4: Siphon off top layer that consists of 99% IPA and let evaporate.

5: Take resulting material and add equal parts Sodium Carbonate (Will Bi-Carbonate work and reach a pH high enough to basify? or should use Calcium Hydroxide?) and make wet (with distilled water) until a paste. Let paste dry until their is no remaining water.

6: Pull off dried paste with IPA or Naphtha and let evaporate for freebased alkaloids.
---If Naphtha is used one could in theory heat it up first (Safely of coarse) then pull off the material and freeze precipitate over the coarse of a few days. Right???

Anyways thank you for any responses! If you have any questions or concerns I am around.

 

[dreamer042]

3: Take 70% IPA and mix into solution pouring the same amount (ml) of vinegar used previously, then add non iodized table salt and mix until the layers separate. (Will the alcohol take in your alkaloids? Are they more soluble in alcohol as compared to vinegar water?)
-Alcohol and water/vinegar are miscible, meaning they mix, you will not get separate layers.

5: Take resulting material and add equal parts Sodium Carbonate (Will Bi-Carbonate work and reach a pH high enough to basify? or should use Calcium Hydroxide?) and make wet (with distilled water) until a paste. Let paste dry until their is no remaining water.
-Bicarb will not push the ph high enough to extract spice. Soda carb and lime both work fine.

6: Pull off dried paste with IPA or Naphtha and let evaporate for freebased alkaloids.
---If Naphtha is used one could in theory heat it up first (Safely of coarse) then pull off the material and freeze precipitate over the coarse of a few days. Right???
-Yes you can freeze precipitate from naphtha.

From what I can tell you are basically attempting to combine a wet tek and a dry tek. I'd recommend sticking with one or the other rather than trying to combine them.

 

[JohnIce2]

Thank you for the reply!
I will more then likely switch to Calcium Hydroxide then if soda wont do.
Also, Isopropyl Alcohol does in fact separate. Basically its 30% water 70% IPA and IPA is not soluble in a salt water solution (I literally just did this in a extraction I did and it worked perfectly separating the 99%IPA at the top from the water + Others at the bottom).

Is their by chance a equation that will tell me the pH of a certain mL of liquid when I add a certain G of a specific base to it??

 

[JohnIce2]

So when this tek was done (With minimal defat, their was still fat in it before basifying. And also no acid added AT ALL) it yielded a red waxy/powdery dust from the 99% IPA that was siphoned off that is very strong to say the least and will post with the Naphtha freeze precipitation results when its finished.

Baking soda can reach a pH of 9. The red/white result was basified enough for smooth vapor (smaller doses in a vape mod). Hopefully that is enough for it to go into the Naphtha.

 

[entheogenic-gnosis]

JohnIce2 said: 2: Defat with Naphtha (Is this Petroleum Ether?)

Synonyms: Ligroin; VM&P Naphtha; Benzin; Petroleum Naphtha, Naphtha ASTM, Petroleum Spirits, Petroleum Ether of varying boiling point ranges from 20 to 75C (68 to 167F)

http://hazard.com/msds/mf/baker/baker/files/p1696.htm

Ligroin is assigned the CAS Registry Number 8032-32-4, which is also applied to many other products, particularly the lower boiling ones, called petroleum spirit, petroleum ether, and petroleum benzine. "Naphtha" has the CAS Registry Number 8030-30-6, which also covers petroleum benzine and petroleum ether: that is, the lower boiling point non-aromatic hydrocarbon solvents. -Wikipedia

Petroleum ethers are extremely volatile, have very low flash points, and present a significant fire hazard.[5] Fires should be fought with foam, carbon dioxide, dry chemical or carbon tetrachloride.[2]

The naphtha mixtures that are distilled at a lower boiling temperature have a higher volatility and, generally speaking, a higher degree of toxicity than the higher boiling fractions.- -Wikipedia

-eg

 

[downwardsfromzero]

3: Take 70% IPA and mix into solution pouring the same amount (ml) of vinegar used previously, then add non iodized table salt and mix until the layers separate. (Will the alcohol take in your alkaloids? Are they more soluble in alcohol as compared to vinegar water?)
-Alcohol and water/vinegar are miscible, meaning they mix, you will not get separate layers.

[...]

I can tell you for a fact that isopropanol does separate out from saturated sodium carbonate solutions, although it'll be 91% IPA (referring to the 99% mentioned in JohnIce2's post) at a maximum, I suspect. With limonene this mixture forms three phases! Or 4 if you count the crystalline sodium carbonate that separates when the IPA pulls some water away with it.

So, saturated salt solution should achieve a similar effect. This will work as an extraction method if the DMT acetate is preferentially soluble in 91% IPA.

Come to think of it, this may indeed be a way of combining the wet tek with the dry tek. Not with the limonene, though.

JohnIce2, I'd suggest removing the plant material before adding the IPA.

Also, you may well be aware that it's very easy to make food grade sodium carbonate by heating dry baking soda in a stainless steel pan until it stops 'levitating'.

 

[JohnIce2]

Thank You for the replies! (And thank you very very much Gnosis for the safety info, will not put naphtha on a heat-plate!)

In all honesty I use this method because it works for me and I am a bit limited resource wise. Basically this method is just the result of a really reallllly dirty extraction I did awhile back (Had Yopo, chaliponga, and syrian rue in about a gallon of Alcohol/Vinegar/Water/Naphtha solution in my waste jar for about a month and this method worked well for me to separate some of the less wanted materials from this into a purer solution. I have no knowledge of a wet or dry tek but I will research them now that they may be of relevance to my current work).

Right now reddish/pinkish/whitish (Three colors here and their) crystals formed from the evaporation of my solution and they have a waxy powdery texture to them (the current one not that waste jar stuff). I didn't quite have the patience to wait for freeze precipitation from the Naphtha so I ended up just pouring it on my evaporation dish with some of the IPA that I pulled from.

Also, the above procedure was not done with any acid at all. I got some Citric acid and Calcium Hydroxide today and I will repeat the procedure using these and get back with the results.
Currently I use a 60W Flood light to heat my evap dish and solutions and it seems to work decently (I reallllly don't want to heat Naphtha with anything else. The way it fumes compared to IPA is much much more drastic and I fear of explosion).

Also on the IPA note, my sources tell me it will be 99%. Check here: Salting Out IPA
And as far as I can tell it does become 99% as I can take a few drops and blow on it for 30 seconds and its gone.

Yet another note (Lol sorry guys, I know its getting long haha), The ACRB I am "Not" using is powdered so their is little chance of me getting it out of solution effectively (unless I use a filter which I do not have right at this moment) and that is initially why I used the "Salt Out" method with my IPA as it limits the amount of residue in the concentrated solvent as the water on the bottom holds the heavier materials while the solvent on top procures your Alkaloids.

After I research what a wet tek and a dry tek are and learn more about the two I may be able to write up a effective mix of the two (Not that we don't have enough teks around here, but I believe creating one that only uses common household materials is desirable and I may put other optional materials in their for a more effective outcome. Not everyone has Xylene or 20% Hydrochloric acid just laying around and purchasing certain materials for extractions just may get one put on a watch list depending on where they are and what all they buy)

 

[JohnIce2]

Quick note: If you for some reason try this method DO NOT VAPORIZE ANYTHING that is left after evaporating the IPA. After the salting out process their is still 1% water that has a minuscule amount of salt in it . Rather use another NP solvent that is not soluble with water or IPA to pull the alkaloids from your solution and proceed to evaporating or freeze precipitating (If you use Naphtha).

Evaporation of the Naphtha by itself yielded small white crystal formations :d .

 

[JohnIce2]

Ok so I wrote this up. Let me know what you guys think. Also theirs a summery at the bottom if you don't want to read it all.

John Ice’s A/B Salt Out Tek

Materials:
70% Isopropyl Alcohol (50% will work but 70% or 91% work better)

VM&P Naphtha (or another NP Solvent that is not water soluable/mercible)

Distilled Water

Powdered Citric Acid (Works best with this because you can oversaturate water solution with Acid to reach a lower pH than the liquid volume allows. Acetic or Hydrochloric acid will also work.)

Calcium Hydroxide (Pickling Lime. Baking Soda and/or Washing Soda can be used in place)

Non-Iodized Table Salt

Dropper/Droppers (Best to have a small one and a medium to large one. I use a 1mL and a 5mL)

Stirring Rod

Measuring Cup (Best to have one that has a spout for pouring on the side. Measured in mL not cups. This is optional and based on personal preference.)

At least 4 Jars with lids (500mL jars work well but may not be big enough for large scale extractions. You could technically do it with less, but 4 is ideal and easier as it gives you work room rather than trying to cramp the entire process into 3 jars)

Evaporation Dish (Optional unless you do not wish to precipitate.)

Freezer (Optional if you do not wish to evaporate)

Plant Material (ACRB, Chaliponga, Mimosa Hostilis, Phalaris Grass, Yopo, etc.) This should work with any and all if done correctly. [Right??]




Procedure:

It is recommended that you read this all thoroughly before attempting as to become familiar with the process. It is rather simple and easy.

Label your jars (either mentally or with a label) #1: Acid Jar, #2: Solvent Jar, #3: Waste Jar, #4: Precipitation Jar/ Solvent Jar 2. Before using any of the above solvents or acids be sure to read up on their individual MSDS forms online as to be as safe as possible. This process can be done relatively fast in comparison to some other teks I have seen. The longest part is the defatting process and Precipitation/Evaporation.
PERFORM THIS IN A WELL VENTILATED AREA!

Step 1:
Take Jar #1. Measure and pour in Distilled Water (Adjust amounts based on plant material used and how much is used. 200mL was used for 18g ACRB).

Step 2:
Take Citric Acid (If another Acid is used that is a liquid replace Distilled Water in step one with it and skip this step). Pour it into the water until a small amount forms at the bottom. Stir solution. If there's still some at the bottom your solution is saturated and you are ready to proceed.

Step 3:
Take Plant Material and dump into Jar #1. Stir until thoroughly mixed. (It is best to use a powdered material. If you are using Mimosa or ACRB that is not powdered then freeze the material and thaw it and powderize before putting it into the acid jar. For Yopo, deshell seeds by lightly roasting them, then grind to a powderish consistency. For Chaliponga, crush leaves into a powder. Powderize all plant material used before this step) Now let your jar with the lid on sit for 30 mins- 1 hour while shaking it every so often.

Step 4:
Take Naphtha (or other NP solvent that is not water soluble) and pour on top of solution in Jar #1. Stir solution. Siphon off Naphtha into Jar #3 and repeat this step until no more plant oils and fats are pulled into the solvent. (This step may require a lot of Naphtha depending on what type of material is used. Some are more fatty than others. If you wish to recover solvent to re-use in this step, stick the waste jar with the lid on in the freezer for a few hours. This should make some of the plant fats precipitate from the solvent where you can remove it or pour the solvent off. The longer and the colder you freeze, the more will come out of it and the more you can put back in).

Step 5:
After defatting is complete take Jar #1 and pour in Isopropyl Alcohol. From here, add Non-Iodized Salt and stir until a layer separates from the solution. (Acid Salt DMT is soluble both in water and Iso. Alcohol so it will migrate into the rest of the solution at this step, more so into the Alcohol.)

Step 6:
Take your Calcium Hydroxide (or Washing Soda. If using Baking Soda convert it to Washing Soda first by baking it in the oven at 400F for a hour.) and pour it into Jar #1 while stirring it in. When the solution is settled and saturated and there is a layer of the basifying agent at the bottom of the jar siphon off the top liquid layer into Jar #2. (DMT Freebase is not very water soluble but is very soluble in nonpolar solvents which means it will migrate almost entirely over to your Iso. Alcohol leaving not much in the water solution if any at all). Put your lid on Jar #1 and put it to the side.

Step 7:
Take Jar #2 and add Naphtha to the solution while stirring it in. Let the layers separate. Siphon off Naphtha into Jar #4 (It is ideal to give Jar #2 a bath in some hot water before adding the Naphtha as to achieve full saturation of the solvent. I personally use a small heat lamp for this step)

Step 8:
From here there are two options: Freeze Precipitate, or Evaporate. This is all up to you and your method of action should be judged on how well your defatting went, how fast you want your alkaloids, the desired formation of your alkaloids, and the NP solvent used (I believe you can only precipitate from Naphtha). If defatting did not go as planned, then go with Freeze Precipitation. If you completed the defatting step completely then you can use either. For Freeze Precipitation put the lid on your jar and stick it in the freezer for 12 hours to a week. The less Naphtha used and the hotter the solution was when it made contact before pulling, the more will crash out and the faster it will do so. If you are getting no results or the beginning of formations after 12 hours, take your jar out, evaporate off half of the Naphtha and try again. For evaporating, pour your solvent onto the evaporation dish and wait. If freeze precipitation is done, one can pour off the solvent back into Jar #2 and repeat steps 7 on until no more alkaloids are pulled.

Summery:
Basically this process is acidifying the DMT (and related molecules) tannin form into that of DMT Citrate then defatting the solution completely, adding Iso. Alcohol, salting that out into a separate layer, freebasing the DMT Citrate (which makes it more soluble in the Iso. Alcohol than the water) and pulling from the solution with a NP Solvent that won't mix with it. You could technically evaporate the Iso. Alcohol and get freebased material but steps 7 and 8 with the Naphtha/ NP Solvent are to ensure their will be no residual salt in the final product. If you wish to vape your final product and not ingest it orally with a MAOi then you need to do steps 7 and 8. If you plan on using oral or sublingual administration then evaporating after step 6 is fine. Burning Salt I beleive releases a chlorine gas which can be really bad for you if not fatal (the 1% of water left in the 99% Iso. Alcohol that is pulled still contains salt and will be in your product unless a non soluble/miscible NP solvent is used to pull the alkaloids from the solution but not the salt).

If you have any questions I would like to hear them.
From those of you who are knowledgeable on the subject of this, would this theoretically work?

 

[entheogenic-gnosis]

So you have not experimented with any part of this procedure in the real world?

-eg

 

[entheogenic-gnosis]

I'll be honest, and I'm not trying to be rude, but I didn't even read through much of your technical work-up, your word choice made it very difficult. I don't mind if there's a misspelled word here or there, or a few grammatical errors, but when the authors linguistic choices make the work-up nearly incomprehensible to the reader I think it's an issue worth pointing out...and again, I'm not trying to be rude, but if I look at a work-up and it's poorly written, I won't even bother reading it.

Here's the other thing,

Most people will put out a technical work-up only after they have mastered the procedure, and fully understand every aspect of it, and only after they have preformed it enough times to be confident in teaching others their method...

When you begin with statements such as:

It is recommended that you read this all thoroughly before attempting as to become familiar with the process. It is rather simple and easy.

and then end with statements like

From those of you who are knowledgeable on the subject of this, would this theoretically work?

it leads me to believe that you have never personally preformed this work-up, and don't fully understand the principles behind it, and thus surely should not be presenting such a work-up in a manner where it looks as if you are directing others to attempt it, or learn from it...

-eg

 

[JohnIce2]

Hello and thank you for the reply!
At the time I posted the extraction tek I had not performed it. I had in the past used several of the fundamental processes that went into this tek tho and with varying success. I do apologize about the grammar and the way it was wrote, the night I wrote that I was not necessarily in the correct state of mind so again, I do apologize. I have since done the procedure and it seems to have worked out fine yielding a tanish red powder and some waxy red (yellow in the light) goo. The process was done with ACRB so I believe the goo to be NMT. When I did post the tek my intentions were not to have someone try it and waste material (if it didn't work) but rather see if anyone found a problem with the chemistry. In the making of it I took the basics of a A/B extraction (which have been previously proven to work by many people) and just added a step that separates the alkaloids from the water layer after you basify the pH. I have no doubt that it does work (to pull something) and I will try my results tonight and get back with everyone.

I am also posting a picture of one of my yields (I have about 3.5g or so of this material and still have not completely evaporated all of my solvent. The 99% IPA layer seems to be so over saturated with alkaloids that their is some at the bottom of the jar. I will freeze precipitate the Naphtha layer to see if I can get any xtals).

Also side note: Entheogenic-Gnosis how would you recommend rewriting it to be more legible? Is it the length or all the parenthesis (I put those in their to note that certain materials used in the step can be replaced with others) or is it rather the lack of exact amounts of materials used?
Again thank you all for your time and replies. I am not trying to waste anyone's resources and until I test the result of this tek to be sure it yields a good product I recommend finding another one for your extractions that is well trusted by and has been used plenty with good results.

 

[Psilosopher?]

A few quick notes on your method.

For your defat step, you must be using a huge amount of solvent. Alternatively, you could use a water bath, and vigorously shake the capped bottle(?) with solvent. If you are not using a bottle, then you could pour it back and forth between two containers to thoroughly mix it. Put it back on the heat bath, and the solvent should rise to the top. The emulsions might take a little while to separate, but it is more resource efficient. You would only need to do this once, instead of using fresh solvent multiple times.

For the heat bath, a temp between 40-60C is fine.

Also, you failed to mention the quantity of raw plant material used. You must be doing a bulk tek to be getting yields of 3.5g, or you're pulling unwanted compounds.

I don't recommend using freshly made base, since it will be hot. Acid base reactions are exothermic, and may push the heat too far. Better to make stock solution, or at least make the base before starting the tek so it has time to cool down.

To answer your question, it can theoretically work, but it doesn't seem as efficient as established teks, especially if you're using bicarb.

 

[JohnIce2]

I do my defeating in a jar at room temperature. I just got done doing another trial of this method on some Chali. and I believe I may have in fact been pulling some unwanted material with the ACRB
Now on the deffating, I believe I am doing it correctly but I may not be. Basically I put in naphtha and then after that I cap the jar, Shake vigorously until the emulsion goes into the naphtha, then I siphon that into the fat jar (Yes I have a jar specifically for it lol. I think I may turn it to soap if that possible). Any remnants of the water solution that get passed into the fat jar through the separation process (I use a 5mL dropper. Very time consuming) falls to the bottom after it has had time to sit and then I collect it and transfer it back to jar I am deffating. For ACRB I used 18g and for Chali. I used 28g.
Side question, does the heat of the acid base reaction destroy the alkaloids at all? I mix the powdered base (for the above I used Calcium Hydroxide) and stir until it gets hot. And boy does it get hot, I mean like burn you when you touch the jar hot.

 

[Psilosopher?]

How long are you letting the mixed solution settle?

The heat does not destroy the active alkaloids. But too hot isn't good either. I range in the 40-60C range and I consistently pull up to 2%. That's why you should let the let the base solution cool down before adding to acid.

Take your time with extractions. The good stuff ain't goin' nowhere.

 

[JohnIce2]

Well for the Chali. it wasn't to long. Maybe about 20 mins or so. For the ACRB I left the first Naphtha pull (for deffating) in for about a hour or two.

By the way: Thank you Bodhisativa!