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Naphtha ? Defatting ? Options
 
quetzalcoatl42
#1 Posted : 6/23/2011 1:18:01 PM
Hi again,

So, I did my first extract a couple of weeks ago, basically following marshfolds tek, but I messed up slightly by not doing several acid cooks, but one instead, kind of misinterpreted the instructions. I thoroughly filtered out any plant material using cotton balls and a t-shirt several times, last time squeezing out as much liquid from the bark as possible. I then let it sit to settle the really fine particles, decanted and filtered the rest of the slug again. The PH was exactly 4, according to my meter. I then mixed a lye solution and poured slowly until the PH reached 12.5 at which point I thought I'd rather not add more, I felt it was enough. It turned gray and then black, as expected. I then used what I believe to be naphtha, but here comes my first question. Where I live you can get two kinds of things, both having the same CAS number 64742-49-0 Naphtha, one is called "Reinigungsbenzin", the other called "Leichtbenzin". The main difference seems to be the length of carbon chains and the boiling point.

"Leichtbenzin" translates to "light-benzin" and it consists of mainly C6 and C7 Hexan free Carbon chains and has a boiling point between 60°-95° C. There is absolutely no residue when evapping a considerable amount repetitively on a clean CD/DVD

"Reinigungsbenzin" translates to "cleaning-benzin" and consists of mainly C7 to C9 Carbon chains and contains n-Hexan. It's boiling point lies between 100°-140° C. Also here, there is absolutely no residue when evapping a considerable amount repetitively on a clean CD/DVD.

Which one is preferable ?

However, I used the heavy one, "Reinigungsbenzin" and hot water bathed my basic solution with the naphtha on top for maybe 30 minutes for the first pull, then 2-3 hours for the second and 24h for the third pull, mixing as well as possible trying to avoid emulsions. Increasing the temperature and allowing gas to get out helped making quite good separations. I used a 35ml syringe to take the naphtha off each time. The naphtha had turned quite yellow each time, especially after the 24h pull. I froze and saw it snowing in my freezer, all looked good. The first batch (1st and 2nd pull) turned out to be quite white, whereas the 24h pull was much more yellow and gooey. So I decided to mix it all up again in a minimal amount of fresh naphtha and re-Xtalize. The outcome was then, to my surprise even more yellow, starting to look even little reddish and wouldnt xtalize so good looking oily and hard to get of the freeze container. So I did that again, worsening the color even further. I evapped the rest of the naphtha after freezing and had to manually xtalize the remaining goo. I regret doing that really, but then again it was my first attempt. The yield was ok, but could have been a lot better.

Since the product was my first smoke ever, I cant really compare, but from what I can tell it was very intense. Starting out with a ringing in my ears, the feeling of all my pores opening and nearly forcing me to cloes my eyes to then for the first time see hyperspace. I'm quite experienced with acid, shrooms and extracted mesc, but the intesity was definitely unmatched.

For my second extract I used twice the amount of MHRB and followed Q21Q21's Vinegar/Lime A/B Extraction Tek. It turned out very well. Also here, I used naphtha, because I am aiming for a smokeable substance and couldn't be bothered to do FASI salting of fumerate solution. I have all the ingredients and I will try next time but for the first dry-lime try I thought naphtha is more easy. The yield was very good. I got EDIT: oops meant to say 2.6g very fluffy powdery white and 0.2g more reddish gooey out of 220g of Bark, although it seems little bit less potent than the reddish spice I made earlier. So here would come my second question. I'm really aiming to get a harder more crystalline product, for that reason I'm really considering doing some defatting on the bark, even though I've read over and over it isn't really necessary.

Would defatting it help getting a less oily more crystalline product ?
How would I de-fat in a drytek ?

If you look at the pictures I took after freezing you can clearly see the oily patches, especially after the long 24 hour pull. Could I avoid those with defatting ?

Thanks in advance

First 2 pulls
http://imageshack.us/f/836/dsc00016ik.jpg/
24h Pull
http://imageshack.us/f/827/dsc00029wm.jpg/
 
ThirdEyeVision
#2 Posted : 6/23/2011 4:13:23 PM
You could:

1) Do the exact same procedure as before
2) Once you salt out your product re-disolve it all in as little diluted acid (ie: vinigar, hcl) as possible
3) Defat that solution with naptha a couple times
4) Then re base it and pull with naptha
5) Salt

There is probably a quicker way to do it at the begining but this should get a fairly clean product.
ThirdEyeVision
It's the third eye vision, five side dimension
The 8th Light, is gonna shine bright tonight
 
Carrierwave
#3 Posted : 6/23/2011 8:46:01 PM
I am running an experiment right now using heptane to pull instead of naphtha. My experiment involves getting my heptane as hot as possible and adding it to MHRB solution that is as hot as possible, because I want to pull as many oils as possible. Granted heptane is a lot more non-polar than naphtha. Then I'm going to start another MHRB batch, but defat prior to basification, and repeat with the same scorching hot solutions/solvents. It was really funny actually, one small shake and it built up so much pressure that when I revealed it at a less-than-upright-angle the solution literally jet sprayed all over my kitchen counter. The result will show my directly if a defat produces anything significantly better. I have Xylene to defat, and I'm also going to hot xylene the bark after finishing pulls with heptane to get the stubborn DMT out.

The longer you leave naphtha in a solution the more it is going to catch unwanted substances like plant oils. The DMT ought to dissolve into the naptha within 10-15 minutes tops if it is a warm solution. Ice cold is a different story. I personally wouldn't try to defat in a dry-tek however, I don't expect the solvent separating very well at all. However that is how a dry-tek works and people have great success with it, I'm just not game to try.
Edit: I just reread Q21Q21 tek, and it says to leave the naptha for 24 hours. I suggest you do Vovin's tek, it's the bee's knee's.

ThirdEyeVision has posted a working technique to recover the DMT from the goo, worth a shot. Also - there is heavy naphtha and light naphtha, heavy is used for defatting, light is used for pulling and re-xing. You could also try to Re-x with a more non-polar solvent like Hexane, or Heptane.
 
quetzalcoatl42
#4 Posted : 6/24/2011 7:35:29 PM
I'm getting xylene now from a pharmacy that ordered it for me, its a liter for 30€, had to tell them I doing a field work on different amounts of taninns in different plant species, they actually believed me... Got all my other stuff from chem supplies, but couldnt find xylene neither toluene. Actually Toluene is being watched in the country I'm from once you order more than 50kg. Checked all the DIY stores for toluene paint thinners but they were all stretched with other oils.

Sounds like a worthwhile experiment you're doing. I usually have the solution and the naphtha medium hot when pouring and then increase the temperature gradually, when I hear the click sound of the jar cap popping out (handy jars) I know I have to release gas. What you were saying sounds exactly like what I noticed. The longer the solvent pulls the more oils get inside. In the drytek I actually only pulled 15 minutes for the first and second and 24 hours for the third. You can clearly see the difference in the color of the spice, didnt mix it this time.

I also did a limo version of the Q21Q21's Vinegar/Lime tek yesterday with 200g of bark and I'm looking at about 4.4g of dmt fumerate now... quite a success. I heard its about 30% more than freebase, will probably convert some after the last pull is completely dry. My limo is as yellow as morning urine. It has been like that from the beginning, ordered it from ebay... Does that matter ?
I'd love to be able to post in the Q21Q21's Vinegar/Lime A/B Extraction Tek forum thread sharing my experiences there. I noticed the dry goo, absorbs a lot more naphtha than limo, especially the first pull, but it doesnt seem to matter the slightest, the yields were great, both ways.
Will maybe try to defat some of the reddish freebase like suggested above, dissolve in vinegar, defat, basify, pull, precipitate. Going to report results, when I'm trying.

Thanks for the suggestions.
peace
 
Carrierwave
#5 Posted : 6/24/2011 8:00:47 PM
I will buy anything off of Ebay if it's on there for a decent price. Urine colored limonene, no idea never used it. Oh wow, a liter for 30 euros! Here in the States we can get a gallon, 3.75 liters or something like that from memory, for 20 dollars (14 euros). Toulene is watched for numerous reasons, one being that TNT stands for tri-nitro-toulene.
 
 
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