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
report on my friend's first extraction ever Options
 
quasimoto
#1 Posted : 11/1/2010 11:38:15 PM
DMT-Nexus member


Posts: 27
Joined: 07-Oct-2010
Last visit: 24-Nov-2010
This experiment was performed, and this report was written, during the third week of August, 2010.

69ron's HCl tek was chosen over his acetate tek for the following reasons:
* the acetate remains waxy instead of forming hard crystals, making it difficult to work with,
* the acetate takes too long to dry,
* the acetate absorbs moisture from the air,
* the acetate is less heat-stable than the hydrochloride, and
* the acetate is less pure after washing with cold MEK than the hydrochloride is after being washed with acetone and isopropanol.

Moreover, to my friend's knowledge,
* more failures have been reported for the acetate tek than for the HCl tek, and
* nausea has been reported more often for the acetate than for the hydrochloride.

In addition, the acetate final product must be produced with MEK, and my friend doesn't know how noxious MEK fumes are.

So the HCl tek was used on ½ pound of HP torch powder. 3 limo pulls were done, each of which then underwent 5 acid pulls.

As a matter of note, the final 2 acid pulls of each limo pull seemed to yield virtually no alkaloids, as the water layers yielded were quite clear, and no transitory emulsions at all were produced. It’s not completely certain that no alkaloids were extracted though, because all 15 acid pulls were then pooled together so they could be evaporated off in a single procedure, and so no attempt was made to observe crude extract yields for each acid pull individually.

Just to verify that all 3 limo pulls were at that point completely exhausted, they were then pooled together, and an additional acid pull was done on that. Upon drying, the tiny amount of residue yielded was green (presumably being mostly chlorophyll) and did not at all resemble the "desirable" crude extracts described below.

69ron states that 3 limo pulls from the cactus powder, with 3 acid pulls from each limo pull, should be sufficient to extract virtually all of the alkaloids. Because of the consensus of opinion (as well as 69ron's personal opinion), and the simplicity of the limo-pull step (seemingly giving little chance for error), my friend is persuaded that 3 limo pulls are sufficient. And because of my friend’s own experience, as well as 69ron's opinion, my friend is further persuaded that 3 acid pulls per limo pull is also sufficient (although some believe more acid pulls may at least sometimes be warranted).

My friend does differ with 69ron on a couple points, however:

1. Contrary to 69ron's assertion that noxious HCl fumes would be given off in drying the crude extract, no such effect was observed. (The extract was dried just by using a fan indoors.)

2. 69ron states that the limo pulls should not be pooled together before undergoing the acid pulls; he says that not pooling them will result in a cleaner product. My friend disagrees. Pooling the limo pulls together will merely have an "averaging" effect - it might be dirtier than the first limo pull by itself, but it will be cleaner than the third limo pull by itself. (Besides, my friend intends to subsequently further refine the crude extract anyway.) And pooling the limo pulls together has this advantage: it requires a total of only 3 acid pulls, rather than 9 (3 for each limo pull). My friend is convinced that this is the way to go in the future.

Upon drying, the crude extract occurred in three essentially distinct forms, listed here in order of increasing (apparent) alkaloidal purity:

Sample 1: Brown (cinnamon colored), and faintly damp, gummy and sticky. It was resinous enough that it couldn't be crumbled to a fine powder, but instead rather resembled pencil shavings (you know, like when you sharpen a pencil). The only sign of crystallization was a few small sparkles after it had been scraped up. There was a slight but noticeable characteristic smell that was a bit reminiscent of downed trees rotting in the forest (which was not unpleasant). It was slightly bitter to the taste. 1.4 grams of this were collected.

Sample 2: Beige (dry milk chocolate colored), dry, and not gummy or sticky. Before being scraped up, it showed crystalline structure but was brown and not transparent. After being scraped up (but before being broken up), it showed some large sparkles. This sample had the same smell and taste as Sample 1, but both smell and taste were very faint. 1.6 grams of this were collected.

Sample 3: Light beige (much like a common color of interior house paint) but with a faint pink cast, bone dry, and not gummy or sticky. Before being scraped up, it showed pronounced crystalline structure and was quite transparent, although it had a slight brown color. After being scraped up, it readily crumbled of its own accord and was then extremely light and fluffy, although the particle size was initially coarse, rather than fine. It had the same smell and taste as described above, but both smell and taste were as strong as that of Sample 1, and stronger than that of Sample 2. 0.4 gram of this was collected.

As has been reported in the "san pedro alkaloids part 2" thread, gas chromatography mass spectrometer measurements indicate that about 60% of the alkaloids removed by the acetone wash (as per 69ron’s tek is done prior to the isopropanol wash) is actually mescaline hydrochloride itself. Because it was thought that that would be wasteful (since mescaline hydrochloride is precisely what my friend wanted to isolate in the first place), it was therefore initially decided to forego the acetone wash.

However, washing Sample 2 of the crude extract with just isopropanol failed to yield pure mescaline hydrochloride, judging by the color of the resultant partially-refined extract. Instead, although enough of the sample was dissolved so that the isopropanol ended up being the color of iced tea (but less transparent, like when sugar is first stirred into tea), the washed product (which was labeled “Sample 2B”) was dried. At that point, it looked to my friend like it was slightly darker than Sample 3, and with noticeably more of a pink cast. (Later, though, my friend couldn’t tell them apart). It was therefore decided to follow the isopropanol wash with an acetone wash, and to try at a later time to recover any mescaline hydrochloride that wound up getting dissolved in the acetone.

First, though, the dried Sample 2B was weighed at 0.9 gram, for a reduction of about 44% from Sample 2. Interestingly, although its appearance was very similar to that of Sample 3, it was about twice as dense, in that the 0.9 gram Sample 2B filled a one-gram vial, while the 0.4 gram Sample 3 almost filled a one-gram vial (when both were slightly compacted).

Meanwhile, the isopropanol used to extract Sample 2B was evaporated to recover 0.5 gram of chocolate-brown, tar-like resin of unknown composition (presumably mostly other alkaloids).

Then Sample 1 was washed with anhydrous acetone. My friend forgot to chill the acetone first, so after putting the sample into it, he put it in the freezer, figuring that any surplus of mescaline that had dissolved in it would precipitate back out when the acetone got good and cold. According to the tek, after two acetone washes the extract is usually very light tan, but it this case it was merely tan (at least wet).

After 2 washes with isopropanol: Sample 1 (now Sample 1B) looked like Sample 2B (except a bit more granular), and weighed 0.6 gram, for a reduction of about 57% from Sample 1. It looked about as light in color as Samples 2B and 3, but was definitely noticeably pinker than both.

Impurities removed from Sample 1, both with acetone and then subsequently with isopropanol were
both chocolate-brown tar-like resins.

Impurities removed from Sample 2 with isopropanol (which yielded Sample 2B): 0.5 gram of chocolate-brown, tar-like resin.

Impurities removed from Sample 2B with acetone (which yielded Sample 2C): very little (0.1 gram?) of cinnamon-colored tar-like resin).

Sample 2C: noticeably paler, pinker (less amber), finer than Sample 3. It lost 0.1 gram (it now weighs 0.8 gram).

Sample 3 first acetone wash (to be followed by isopropanol washes): paler, pinker than Sample 2B; still 0.4 gram left. After 2 acetone washes: not noticeably paler or pinker; now @ 0.35 gram.

Impurities removed from Sample 3 by both acetone washes: cinnamon-colored resin, NOT tar-like, about 0.1 gram.

Sample 3 underwent 2 acetone washes and 2 isopropanol washes (not dried in between 2 isopropanol washes).

At this point, all samples were dry powders, all pale pink (with a slightly amber tinge).
 

Explore our global analysis service for precise testing of your extracts and other substances.
 
 
Users browsing this forum
Guest

DMT-Nexus theme created by The Traveler
This page was generated in 0.023 seconds.