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colored naptha after pull?

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dtabbler

dtabbler

Rising Star
first let me say this is swims first time using mhrb powder from a known good supplier, he did one quick pull on 3650ml filtered h2o, 240g bark powder and 240g lye. these results were great! 1.5g!

He then added some fresh naptha and let sit a few days rolling and shaking and moving periodically, heated the mixture in water bath to 50C and pulled again, also very successful at slightly over 900mg. Then he added the left over naptha from his first pull (something he'd never done before usually leftover naptha after a freeze precip is put in a separate dish and evaporated to be sure any leftovers are gotten) and left the jug to sit overnight in the warmest spot in his temple.

heres where something funky happened... he pulled the jug out of the warm place (22-25C as opposed to the usual 17C he keeps it) and noticed the naptha had alot of color and was very cloudy almost fatty/oily looking. he went ahead and heated the mixture to 50C in water bath and pulled, freeze precip yielded an odd yellowish/orange color crap that looks worse than what he's used to seeing with xylene even!

The question is what did he do wrong? he feels this is from the used naptha but is unsure.

also he would like to note that when the naptha was added it was room temp and was added to 50C solution. is this the problem?

he's not sure whats in this cloudy mix yet as he is letting it naturally evap and will re-xtal with naptha tonight (doesnt wanna waste heptane on something he's not sure about!)

fortunately he's happy with the results from the first two pulls but knows there should be more spice hiding in there! he's adding xylene to the jug tonight and going to let that sit a few days.
 
STB + Prepowdered back can sometimes pull some strange colored compounds. Very hard to get rid of save a small scale A/B extraction on your final STB goop.

Many things have been tried, washes, rextalizations, etc...nothing has worked so far that I am aware of except doing a mini A/B.

I hate STBs
 
swims never had a problem like this before. but have never used prepowdered bark either.

note: he's only done about 12 or so extractions
 
Throw it in the freezer for a little while and the cloudy stuff will settle on the bottom, then decant into a new container and continue your work.

Pokey
 
unfortunately that was the problem pokey even after a freeze it remained consistent.

tried to recrystallize with naptha, turned worse.. what was a dried up, orangey, dirty dmt from xylene consistency item turned into a very wet gelatin like burnt orangey goo.

swim going to other methods of relaxation for the night
 
Hi dt, I had a problem recently where my naphtha was a weird cloudy brown color (first time ever). I pulled it and placed it in a jar for a little while. Amazingly the cloudy brownness went away leaving a brown layer right on the bottom allowing me to pull the yellow naphtha off the top. I tossed the brown yuck away. I froze the yellow naphtha after evapping it a bit and some decent yellow stuff started precipitating. A rexlzation will make it nice and clean, but i was wondering if this what you were experiencing? Any luck getting the goods out of the mess?
 
doingkermit, wish i would've read that before, what was done is: freeze precip the whole brown cloudy mixture, the brown solids sank to the bottom and the naptha was poured off into another dish to naturally evap. the dish with the brown gunk was scraped up, then an attempt at a rex was made with naptha.

the warm naptha was added to the warm gunk and was not doing a good job at dissolving it, also noted the brown gunk did not melt in 48-50C water bath. A large amount of naptha and stirring was involved in getting the mixture liquefied, approx 40-50ml, this was then set aside to slowly cool to room temp (it's cooled in the water bath so it cools VERY slowly) during the process the gunk stayed in the mixture but in liquid form :(

so now there is a beaker of brown jelly that needs to have something done with it yet swim is not sure what to do. he has yet to look at dish B which has the poured off naptha from the freeze precip although one would be quite certain any goodies would have stuck in the goop.

the thought is to do a small scale a/b as acolon_5 mentioned, and re-evaluate the rest of the prepowdered bark and what to do with it as this was kind of a small test on new material. swim has had great luck with STB before this experience and feels the a/b involves more work the necessary, but may have to result to it in this case. Honestly, why go A/B when STB works well and involves less work? some claim they prefer due to "hazardous materials" used in STB, but any goodies that are for use after STB have always undergone a min. of 4 rextals in swims presence (with the exception of his first extraction) and he feels that is more the sufficient at removing impurities.

swim is also curious, this problem only arose AFTER heating the mixture, is heat not needed with pre-powdered bark? the first pull was done at room temp, the second pull the jug had sat at room temp until pulling time at which point the mixture was put in hot water bath until temperature reached 50C, he then pulled the naptha, added the old naptha from the first pull and set aside. Heat has always been saved for the last few pulls during every other extraction he's done, but felt it would be beneficial this time.
 
Yea this brown naphtha PISSED ME OFF because it happened to me on my VERY FIRST attempt of a DMT extraction...

Sodium carbonate cleanings worked miracles for me when i had brown naphtha, and i did several cleanings until it went clear enough to freeze, and i did a re-xstal on the dmt it froze to FULLY clean it....Worked perfect for me....I only do whole bark with STB because of this....Pre-powdered calls for a good A/B tek that needs simmering and filtering....

If a few sodium carbonate washes don't clear it up, just do a mini A/B extraction on the brown gunk.....
 
Yeah.. A/B it, man. Sounds like you are at the stage where you don't have many other options unfortunately. I have never had this brown naphtha dilemma until recently. Keep us updated, man. Would be cool to hear how it turns out. Peas
 
killuminati420 said:
Yea this brown naphtha PISSED ME OFF because it happened to me on my VERY FIRST attempt of a DMT extraction...

Sodium carbonate cleanings worked miracles for me when i had brown naphtha, and i did several cleanings until it went clear enough to freeze, and i did a re-xstal on the dmt it froze to FULLY clean it....Worked perfect for me....I only do whole bark with STB because of this....Pre-powdered calls for a good A/B tek that needs simmering and filtering....

If a few sodium carbonate washes don't clear it up, just do a mini A/B extraction on the brown gunk.....
Click to expand...

Thanks! will try this next time, another thought that popped into my mind was possible an activated carbon/charcoal whatever it is wash if anyone has thoughts on that?

Also swim would recommend multiple rextals on any STB tek especially! if you've ever done repeated rextals you'll notice you don't leave much behind on time 3 and 4 but there is typically about half the contaminates of time one on time 2 (example: you get 50mg of garbage out the first rextal on the second expect to still get 25mg of garbage, 3,4, and more produce diminishing returns)


DoingKermit said:
Yeah.. A/B it, man. Sounds like you are at the stage where you don't have many other options unfortunately. I have never had this brown naphtha dilemma until recently. Keep us updated, man. Would be cool to hear how it turns out. Peas
Click to expand...

heres some photos of the gunk and the jug that now has xylene in it, notice the chocolate milk appearance of the xylene, not sure whats going to come of that.

on a good side note, Dish B previously mentioned containing the naptha that was remaining from the freeze precip attempt naturally evaped some interesting looking crystals.
 

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The bottom pic is sideways. The bottom layer of mhrb/lye/h2o is on the right, xylene on the left.
 
I got coloured naptha on my first extraction but after letting the goo settle after each pull the naptha was decanted into a new container and the naptha was pretty clean.

I'm wondering if the vigorous shaking that is done in nomans and other teks could be responsible for this transfer of orange colour in the naptha, maybe just letting the mhrb soak in the basified water without shaking would make a difference or is the vigorous shaking necessary?
 
De, that's exactly what i was saying i did... and it worked a treat! Not sure if the shaking vigorously thing is the problem. I think it is necessary to do it before adding the solvent to allow the sodium hydroxide to break down the bark even more (even if it is powdered). Then after the solvent (naphtha) is added, a light shake and rolling around over and over is a better way of retrieving the goods, without creating silly emulsions. Why the naphtha turns brown/red is weird and for some reason i don't think it is from emulsions which is causing this. I am not a scientist, so i don't know for sure what is making the unknown brown stuff enter the solvent. Thanks for the imput tho, man.

Lots of peas :)

DK
 
Cheers kermit :D swim is doing another extraction this week and his mhrb is from a different supplier, we shall see if this coloured naptha problem persists, i shall let you know ;)
 
Shaking is bad from the point where the mixture is basified on, in my experience. I suggest gentle rolling from then on.
Also as a last resort, if you have stubborn goo and don't know what to do with it, add it to your next extraction.

Pokey
 
-_-° SWIM got some very dark naptha too, damm.....
Yesterday SWIM tryed the 2kg extraction from The DMT Handbook with some prepowdered MHRB, his very first extraction btw. Why the f..k to start with a bulkextraction?! Because he thought he knows what he was doing and this tek sounds sooooo easy to him :D.... A lot turns wrong but nothing serious (lucky to had a little clue what to do and not only "cooking some recipe"). After SWIM added 5l acidwater to the bark and got just a kind of mash he decided to divide it to work with. The bigger part was given to a large jug, filled with some more acidwater and placed aside to do a cold extraktion for A/B (2l nice red acid was collected yet, Jug was refilled). The other bark was tryed to simmer but scorched on the bottom of the pot a little bit. SWIM tryed to filter but it caulked the silk. He put all in a clean jug and did an STB with 250g of lye... ok ok its an FATB :/ SWIM pulled with 3x330ml naptha and yes, to his blame he shaked very well. He evaped 5ml of the brown naptha and ended with the same blackish brown goo...
SWIM is now going to acidify the naptha, add some water, remove the contaminated naptha, basify the water and does another pull with fresh naptha... is he on the right side with it?
I'll add some pics if SWIMs work is done. Is there allready a tek for this prob?
MFG Mindbender
 
Swim added vineager to the goo (acidified) pulled the vineager off via sep funnel, then basified to ph 12-23, added xylene then pulled X2 with results similar to what was expected. Turned out a very clean product.
 
SWIM thinks it might be from such finely powdered bark. If you shake the container hard with finely powdered bark, tiny particles may get suspended in the naphtha. Judging from the fact that separating it, and letting it sit, the brown drops out, it's probably tiny bark from such fine powder. If one shakes a little less, and/or lets it completely settle, perhaps it wouldn't come out as brown naphtha. In SWIM's tek, he often gets yellow naphtha with lots of color, but it's never brown. The DMT is easy to recrystallize from it, and he can save some yellow/orange type stuff and the pure white, for some variety.
 
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