We've Moved! Visit our NEW FORUM to join the latest discussions. This is an archive of our previous conversations...

You can find the login page for the old forum here.
CHATPRIVACYDONATELOGINREGISTER
DMT-Nexus
FAQWIKIHEALTH & SAFETYARTATTITUDEACTIVE TOPICS
First Mescaline Extraction Results Options
 
Pennyless_Sitar_Player
#1 Posted : 11/28/2010 9:13:37 PM

DMT-Nexus member


Posts: 51
Joined: 28-Nov-2010
Last visit: 26-Jun-2011
Location: The Rouge
Hi guys,

While in a restaurant the other day, I overheard a conversation where this guy described for his friend his first mescaline extraction, and I thought it might be of interest here. He also mentioned a url where he had uploaded some photos. Luckily I was able to retrieve copies of those before I lost the url.

He started with 5.8 lbs of san pedro cactus. This was sliced thinly and dehydrated over two days in a couple of food dehydrators. Then, the slices were ground in a coffee grinder to result in 158 grams of fine powder. He mentioned nothing of skinning, de-spining, or removing the core. He just dried and ground the whole thing.

Next, he placed the powder in a two liter wide mouth glass container (like a beaker) and added 1.4 liters of distilled water. This was mixed five times, five minutes each, over a 50 minute period with a hand-held blender clamped to a supporting rod. It was mixed in intervals to let the blender cool - five minutes on, five minutes off.

With the water and powder thoroughly mixed, he began slowly adding sodium hydroxide while blending. Again, this was done in five minute intervals over the course of an hour. A total of 395 grams of sodium hydroxide was added - 2.5 times the weight of the powder. I know, this seems excessive. But he explained that it was being used to break down the cell walls of the cactus powder, in addition to raising the pH of the solution. He thought of it as being similar to clearing out a drain, where copious amounts of sodium hydroxide are used to break down plant matter- roots and such. He thought that an excess of sodium hydroxide would break open the cells and liberate the alkaloids, which would then suspend freely in the basic solution. He allowed this basic solution to sit for 48 hours, blending it periodically for 5 minutes at a time.

At this point, he described the solution as completely liquefied. He started the blender and added 300ml of xylene, which he allowed to blend for 5 minutes. Interestingly, the blender imposes a vigorous, yet smooth, stirring action that does not result in much emulsion forming - though there was some. He waited five minutes, then stirred three more times for five minutes each. He then placed the beaker in a hot water bath, which was in the form of a stainless steel cooking pot sitting on a hotplate filled with enough water to raise the level just over the level of the xylene in the beaker. The water temperature was monitored with a thermometer, and kept at about 40* Celsius for about 3 hours. The heat was turned off and the mix allowed to settle over night.

The next day, he found a distinct three layer separation in the mix. The bottom layer was about 100ml, and was very dark brown, similar to the waste layer one would find when defatting. The middle layer was about 1050ml of green liquid, same color as the basic solution he'd created. The top layer was about 250ml of dark amber, almost orange, clear liquid. The interface between the green and amber layers was fairly clean, no significant emulsion. He assumed the top layer had the alkaloids, so that was drawn off with a vacuum. He described the vacuum device as flexible 5mm Teflon tubing connected to a side-arm flask via a single-hole stopper, and the flask connected to a hand pump with standard vinyl tubing. The flexible Teflon tubing was stiffened by passing it through a 1/4" copper tube. The copper tube was clamped to a supporting stand, and the flex tubing slowly pushed through it into the xylene - being careful not to expose the copper to the xylene.

The extraction went quickly with a few pulls on the pump, but he did end up pulling some contaminants from the green layer. He poured the contents into a jar, and cleaned sidearm flask with acetone. He then filtered the xylene through a buchner funnel fitted to the sidearm flask and using medium filter paper, using the same vacuum to pull the liquid through. The result was a very clean, 250ml amber xylene product, and clearly visible contaminants on the filter paper - which was discarded.

The xylene extraction was repeated four more times using precisely the same steps, including the filtration - he just couldn't avoid pulling contaminants through the vacuum. After a while though, he didn't care about them because the filtration step was so effective at removing them. He noted that the fourth and filth extractions yielded xylene products that were increasingly lighter in color, the final one being a yellowish gold color - much lighter than the original dark amber.

He now had about 1500ml of amber xylene, which he poured back into his 2 liter flask (after cleaning it of course). He then poured 300ml of distilled water into a separate flask, to which he added enough HCL to bring the pH down to around 2 - a cheap digital pH meter was used. The xylene was set on a magnetic stirring plate and brought to a gentle stir with a medium size stir bar. The acidic water was slowly added to the stirring xylene, which was allowed to stir for 30 minutes. After stirring, the mixture was allowed to sit for 5 minutes. It separated into two layers with a considerable white emulsion between the two, about 50ml worth of emulsion. The mixture was placed in a hot bath at 40*C for three hours. Periodically during this time (about every 20 minutes), a glass stir rod was used to gently stir the top layer and the emulsion at the interface, which was gradually dissipating. After three hours the emulsion was gone.

The mixture was gently poured into a 2L separating funnel and allowed to sit for 30 minutes, after which there was a clean separation with the water sitting below the xylene. About 5ml of water was drained off as waste in case any xylene was trapped at the stopcock, and the rest of the water was collected and set aside in a mason jar. He then proceeded to repeat the water extraction four more times, ending up with roughly 1500ml of water.
He mentioned two things here that caught my attention. First he said that emulsions are tough to work through, but doing so is a worthy trade-off to getting a good thorough mixing. Thorough mixing is important at all phases of the process, he believed. He said he that the alkaloids migrate across phases only when they are in physical contact with the target phase, and that only happens during mixing or stirring. His advice was to keep the stirring as smooth and gentle as possible, but to let it proceed over extended periods of time. The second thing he mentioned was that dealing with emulsions is easier in beakers than in seperatory funnels, because gently stirring or breaking up the emulsion with a rod helps it dissipate faster, which is a lot easier with the beaker's wide mouth.

He then poured the water into a large Pyrex baking dish and let it sit in front of a box fan running on medium to evaporate the water. This took about 36 hours he said, after which he found tan colored residue in the dish. He scraped this up with a glass scraper and weighed it at 1.24 grams. Under the microscope there was a combination of very small clear, white, and tan crystals, many shaped as needles, some like flakes. They were a bit sticky or oily to the touch. The taste was bitter, with a slight numbing affect to his tongue.

He decided to try and clean up the product to see what would happen. He placed the product in a small beaker and added 100ml of dry acetone. Using a glass rod, the product was ground finely, and then the mixture was allowed to stir magnetically with a small bar for 10 minutes. The mixture then sat for 3 hours while the solids settled at the bottom. After this, the acetone was poured off being careful to not disturb the solids. This was repeated twice more, then the the solids poured onto a glass plate and allowed to evaporate, which only took 30 minutes in front of a fan. The result was a 1.21 grams of a tan product that was not at all sticky or oily. The acetone waste that was poured off was allowed to evaporate also, yielding an oily, green and yellowish residue that never really dried. He still didn't know what that was, but it was obviously a containment and was discarded.

Now, he wanted to try separating the mescaline from the other alkaloids - san pedro cactus evidently has several other alkaloids. He placed the product back in the small beaker and added 100ml of 99% isopropyl alcohol. This was allowed to stir magnetically for 10 minutes, then settle. The alcohol was poured off being careful not to disturb the solids at the bottom, then the product was emptied into a glass dish to evaporate. The alcohol that he poured off was also allowed to evaporate. The product dried to reveal 804mg of bright white powder, the alcohol evaporated to leave 398mg of darker tan powder. He said both had a crystalline quality, and look very crystalline under the microscope. There is a preponderance of needle-like shapes in the white product. The tan product also has some needles, but is mostly flakes. He noted that the white product tasted bitter, and the tan product was bitter but with a noticeably greater numbing sensation. He thought further separation was possible, but chose to stop at this point.

Attached are the photos I pulled from his url before i lost the napkin on which i had jotted it down. The first shows the initial 1.24 grams of product. The second shows the white and tan products separated. The third shows the strange yellowish green goo that was washed out with the acetone.







Pennyless_Sitar_Player attached the following image(s):
IMG_0609.JPG (18kb) downloaded 118 time(s).
IMG_0617.JPG (37kb) downloaded 118 time(s).
IMG_0644.JPG (24kb) downloaded 118 time(s).
Everything contained within this post is pure fiction, written from a character's perspective within the author's mind as he dreams aloud... come what may
 

Good quality Syrian rue (Peganum harmala) for an incredible price!
 
Noman
#2 Posted : 11/28/2010 9:30:38 PM

DMT-Nexus member

Senior Member

Posts: 1052
Joined: 18-Jan-2008
Last visit: 30-May-2021
Really nice work and a great write up.
One has found that adding salt to the initial aqueous solution and doing an NP wash on the xylene helps prevent emulsions - though they didn't seem to give that much of a problem here.
Did this guy mention why he chose HCl over H2SO4 for the salting step?
 
Pennyless_Sitar_Player
#3 Posted : 11/28/2010 11:14:30 PM

DMT-Nexus member


Posts: 51
Joined: 28-Nov-2010
Last visit: 26-Jun-2011
Location: The Rouge
Thanks. I believe he mentioned HCL was used because he had some on hand. Is there an advantage to using H2SO4?

Also, thanks for the tips on dealing with emulsions. Great info. Do you know where to find specific steps on the NP wash of the xylene?


Noman wrote:
Really nice work and a great write up.
One has found that adding salt to the initial aqueous solution and doing an NP wash on the xylene helps prevent emulsions - though they didn't seem to give that much of a problem here.
Did this guy mention why he chose HCl over H2SO4 for the salting step?

Everything contained within this post is pure fiction, written from a character's perspective within the author's mind as he dreams aloud... come what may
 
Noman
#4 Posted : 11/29/2010 12:17:01 AM

DMT-Nexus member

Senior Member

Posts: 1052
Joined: 18-Jan-2008
Last visit: 30-May-2021
Pennyless_Sitar_Player wrote:
Thanks. I believe he mentioned HCL was used because he had some on hand. Is there an advantage to using H2SO4?

Also, thanks for the tips on dealing with emulsions. Great info. Do you know where to find specific steps on the NP wash of the xylene?



I don't know. That's what I was wondering about HCl.

It's just like a DMT NP wash. Before you salt, mix your NP with about half it's volume of pH 11 or so aqueous solution.
 
DiMiTriX
#5 Posted : 11/29/2010 10:12:29 AM

DMT-Nexus member


Posts: 664
Joined: 07-Sep-2010
Last visit: 14-Nov-2016
Location: europe
really nice pictorial tek man,thanks a lo,really clean product too
Tz'is aná
 
Pennyless_Sitar_Player
#6 Posted : 11/30/2010 1:43:52 AM

DMT-Nexus member


Posts: 51
Joined: 28-Nov-2010
Last visit: 26-Jun-2011
Location: The Rouge
I've done some checking around and haven't been able to find any qualitative differences between the HCL and H2SO4 approaches. There are some physical differences - weight, melting point, etc... but apparently, they clean up the same and offer the same experience. Dosages are different of course, because of the weight variance.

I don't think there is an advantage to either - or at least I haven't found one yet.


Noman wrote:
Pennyless_Sitar_Player wrote:
Thanks. I believe he mentioned HCL was used because he had some on hand. Is there an advantage to using H2SO4?

Also, thanks for the tips on dealing with emulsions. Great info. Do you know where to find specific steps on the NP wash of the xylene?



I don't know. That's what I was wondering about HCl.

It's just like a DMT NP wash. Before you salt, mix your NP with about half it's volume of pH 11 or so aqueous solution.

Everything contained within this post is pure fiction, written from a character's perspective within the author's mind as he dreams aloud... come what may
 
Pennyless_Sitar_Player
#7 Posted : 11/30/2010 1:46:41 AM

DMT-Nexus member


Posts: 51
Joined: 28-Nov-2010
Last visit: 26-Jun-2011
Location: The Rouge
Thanks man. I'm sure this was a lot of fun, and very educational.

DiMiTriX wrote:
really nice pictorial tek man,thanks a lo,really clean product too

Everything contained within this post is pure fiction, written from a character's perspective within the author's mind as he dreams aloud... come what may
 
ouro
#8 Posted : 11/30/2010 2:02:27 AM

DMT-Nexus member

Moderator

Posts: 596
Joined: 09-Sep-2010
Last visit: 25-Mar-2024
Very detailed write up, Pennyless... It looks like you did a fine job. M sulfate salts have very low solubility in cold h2o so they are easier to recrystallize and get pure mesc. But, sulfuric acid doesn't evaporate like hcl so proper titration is more important. Hcl is usually easier to get, too.
 
Pennyless_Sitar_Player
#9 Posted : 11/30/2010 3:43:04 AM

DMT-Nexus member


Posts: 51
Joined: 28-Nov-2010
Last visit: 26-Jun-2011
Location: The Rouge
Ahhh, i see. Thank you ouro, this is good to know. I have a lot of reading ahead of me here.


ouro wrote:
Very detailed write up, Pennyless... It looks like you did a fine job. M sulfate salts have very low solubility in cold h2o so they are easier to recrystallize and get pure mesc. But, sulfuric acid doesn't evaporate like hcl so proper titration is more important. Hcl is usually easier to get, too.

Everything contained within this post is pure fiction, written from a character's perspective within the author's mind as he dreams aloud... come what may
 
dg
#10 Posted : 12/4/2010 9:30:11 PM
DMT-Nexus member

Cacti expert

Posts: 1175
Joined: 10-Jun-2010
Last visit: 27-Apr-2016
Pennyless_Sitar_Player wrote:
I've done some checking around and haven't been able to find any qualitative differences between the HCL and H2SO4 approaches.


if accurate titration is used,
sulphuric acid form spectacular crystals- but dont titrate to ph 2, you will have acid left over that wont evap away like hcl (the main advantage of hcl....)
ph 5-6 is about right, with ph 7 getting 95% and less impurities
 
 
Users browsing this forum
Guest

DMT-Nexus theme created by The Traveler
This page was generated in 0.049 seconds.