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Re-x to only remove the brown

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tracid1987

Rising Star
Hello folks

I have recently done an extraction from MHRB.i got 2% yield. What is strange that since the first pull i got light brown crystals and every other pulls gave me light brown crystals as well.i could dry them up quick perfectly without any sticky stuff.
I dont know why i got that light brown colour. My naphta is clear, and i also was very cautious when pipetting the nps solvent from the soup so the crystals are without any toxic contamination. I suspect pigment from MHRB. That isnt big problem since it can be vaporised but the brown stuff leaves a black burned stuff behind which often gets into my mouth together with the vaporised DMT which is a bit annoying.

I am not a big fan of re-xing since i dont want to loose 40% of precious material- i am sure there are other stuff in there which have synergistic effect together with N,N-DMT but it would be nice to remove that light brown stuff from it.

If i use heptane i will get white crystals but with significant loss of yield.

Is there any method to deal with that light brown stuff/pigment? To do a less effective re-x so i remove the brown only but leave the other precious material?

Thank you very much
 
I bet if you dissolved your spice with hot naphtha in a shot glass, as it cools all your brown will fall down to the bottom and stick. You can decant the liquid and then once you dry both you’ll have a pile of cleaner spice and a pile of brown to do with whatever you like.

Complete side question, you think that brown would be good on changa?

If it is somehow lye bark sludge you gotta get rid of that, I don’t know how spice burns but if plant fats don’t do that same burning to black then you need to do a mini a/b to get that out.
 
It's probably just some plant matter. The 'adulterant' might even be active (look up "jungle spice"...) I think people are waay too much hung up on getting white crystals.
 
Brown is weird. I would be careful and purify.

Re-x doesn't have to mean loss of yield. You can re-x once and then re-x the waste again with just a part (anything between 1/2 and 1/5 dependent on the impurities) of the initial solvent, and continue till it makes sense (yields dmt).

If done correctly, re-x yields two or more fractions, there is no loss in fact. If you just want pure spice for vaping/smoking, get as much of pure dmt as possible (3 cycles?) and then use the waste (impure fraction) in next extraction.

Heptane is suggested. Heat it as much as possible make it as saturated with dmt as possible. Then let to cool down to desired purity (by color of heptane - something between 50C and 20C). When hot, it's colored and while cooling down, it is losing the color. Once happy with color, just pour away to another beaker and freeze.
Repeat with less heptane again.
Repeat till makes sense (yields dmt in reasonable amounts).
 
I recently pulled red/brown spice from mhrb using naphtha. My naphtha turned dark though, you nearly could not tell the difference between the layers of basic and solvent. Searched the nexus, found this is not without precident. I did a bioassay and my rust colored spice placed this grateful little human into the hands of the Source. I think next extraction I will use xylene.
 
It's my understanding that 'naphtha' can mean a pretty wide range of hydrocarbons, from light to heavy. There's 'Wundbenzin', 'Waschbenzin', lighter fuel, petroleum, etc. These all vary in how selective they are in their pulls...

That said, if there's some solid ash or other stuff flying into one's mouth when smoalking, I agree that it's probably better to clean it up. (Or maybe use a different smoalking setup, like a balloon vaporizer.)
 
Yes, this is true. But selectivity of any of them can hardly be compared to toluene or xylene.
I always do initial extraction by toluene and then purify by mini-A/B with re-x by heptane. A lot of color stays behind the purification.

I like to stay on the safe side. Because nobody knows what this color is, it is safer to purify. Especially for vaping/smoking. Mini-A/B with hot heptane pulls and re-x should fix this.
 
Thank you all for replying :)

I will try to clarify in more detail:
So i was using STB method. I was using lab grade Petrolether as solvent (nothing left after evap test). and NaOH for making soup. This was my 2nd extraction.
At the very first extraction i got yellowish spice.
At the second extraction i got light brown spice (very light sandy colour), heres the pic:
https://imgur.com/a/mcMGkZG
Only the source MHRB was from a different purchase (but the same vendor, the same product).

I am not drawn to white crystals at all, even not tried white yet. if i know that the yellow or brown spice is richer in alkaloids then i prefer them. This is why i wrote i dont want to re-x if not needed.
What is worrying me is the black burned stuff flying into my mouth when vaporising and i bet it is the brown stuff burned. I know that cannot be any lye, i was very careful during the process. That is some kind of plant material.

But i was afraid of re-xing due to loss. But i might try like pete666 suggested (thank you pete666).

i was curious if there is any method to not fully re-x the spice, only like partially removwe impurities.

Would a mini A/B on the spice help? Or a simple wash with water? If i dont do mini A/B but a simple water wash i think theres no need to add NaOH, just water to the spice then solvent, am i right?
 
Can you point me to a mini a/b description,please? coz its not in the faq section, i have found one topic but its not completely clear for me how much vinegar,nps,naoh,water/spice to use.

At my very first extraction i made a sodium carbonate wash but i am not doing it any more. i had a significant loss of yield by washing with sodium carbonate and somebody wrote here that it is possible to loose spice by this. so there is no way i will attempt it again.

After that when i performed a mini a/b i got three layers, not two, it was very strange, look:
https://imgur.com/a/38CiXR0
.
So i am afraid of mini a/b again this is why i would need more complete instructions how to do it.
I would be very grateful (the steps are clear to me just the ratios i dont know).
 
It should be somewhere, but here is how I do it. Ask if anything unclear...

Take dmt freebase and weigh it.
Fully dissolve it in hot naptha, use about 30-40ml per gram of dmt. Add 1/3 of water compared to naptha. Heat up, you don't want boiling naptha, but it should be really hot. The temperature helps to avoid emulsions.
Then salt it. Simply add acid, so all dmt is converted to its salt form. In this calculator you can see pH you have to achieve to be fully salted. pH 6 is your target, but can be lower, no prom.
For every acid the amount is different, I am using 3,7% HCl and each 1g of dmt freebase requires 4,36ml of the acid.
Mix thorougly, so dmt can transform. I am using either erlenmeyer flask or closed bottle and mixing as much as possible for few minutes. Then measure pH of water layer (thin pipette), if basic, add more acid. If acidic, mix again for few minutes and check pH again. If still acidic, you are there.
You don't have to measure the pH if you don't want to, you can simply add enough acid, even much more than necessary. You just have to add enough base later in that case.

Once salted (pH6), separate water and discard naptha (can be used for next extractions).
Add NaOH to the water. I usually add a plenty of it, much more than necessary. I just don't care. Once I didn't add enough and almost lost some dmt. You can target pH 11-12 (see the calculator), but if it's more, no problem.
The water should get cloudy.
Add heptane, 20-30ml per g of dmt.
Heat up again (70C).
Mix like crazy for few minutes
Separate hot heptane. If you are using pipette, it is good to heat it up before pulling by pure hot heptane, so dmt does not crystallize inside cold pipette.
Pour saturated heptane into beaker.

Repeat pulling with half of the heptane again, combine pulls. If makes sense, repeat again with half of the heptane. Keep the beaker with pulls hot if you want to re-x.

Once all pulls done, either freeze-precip the beaker in the freezer or do re-x as stated in some of my parevious posts.

Please make sure everything makes sense to you before you do it. I might have made mistake, writing on the fly :)
 
Yes it makes sense. Thank you for the detailed procedure. Especially the ratios/amounts-calculators are very important to me.You helped me a lot.

Where you wrote "water" i think you meant the acidic solution, right? because you do not add water, right?

Isnt better to use petrolether instead of heptane? i mean i didnt want white crystals, i prefer the full spectrum. but if i use heptane it is kind of like i re-xed alredy in one go.

by the way, did you check the link in my previous post? why did i have three layers during the mini a/b? (unfortunately i cant remember exactly how i did it, it was my first attempt)
 
No problem

tracid1987 said:
Where you wrote "water" i think you meant the acidic solution, right? because you do not add water, right?
Click to expand...

When you have naptha with dmt freebase, distilled water is added and then acid. So water is added, but then it becomes acidic solution with dmt salt dissolved. OK?

tracid1987 said:
Isnt better to use petrolether instead of heptane? i mean i didnt want white crystals, i prefer the full spectrum. but if i use heptane it is kind of like i re-xed alredy in one go.
Click to expand...

Do you want full-spectrum? Then yes, you can use naptha. But HOT heptane takes a lot of "orange" too. It is all question of at what temperature point you use the heptane. If you have it fully saturated at 70C, you get nice spectrum, not just white dmt. If you let it go to 25 and use it from there, it is almost white.

tracid1987 said:
by the way, did you check the link in my previous post? why did i have three layers during the mini a/b? (unfortunately i cant remember exactly how i did it, it was my first attempt)
Click to expand...

Yes, looks like classic emulsion. Heat should solve it.
 
it took a while because i didnt have much time for this.so today i wanted to do a mini A/B as you suggested.


I again got that emulsion:
https://imgur.com/a/tiqKPyJ

I am heating the NPS+dmt+water+vinegar solution for a while now but the emulsion seems not disappearing.

Do you have any advice how can i completely neutralize the emulsion?

btw thank you for your instrucions, i appreciate them.

Thank you a lot
 
When i have added the water i shaked it gently only so no emulsion has formed. but after i have added the vinegar it started to get cloudy- i mean that third layer in between.after shaking it was bigger.

its no problem for me to pipette off the solvent with the white emulsion then discard if i cannot reuse it due to the white emulsion. so if you tell me i can proceed with the lower layer then i will basify it and proceed...

i just cant understand why is that white layer still there. i was even heating it for more than a hour

Note: i dont know if i can add non-iodised salt to break the emulsion. i know it can be used in the basified soup but dont know if i dont damage anything if there is vinegar in it as well
 
I just don't understand why your water layer is so high? The suggestion was to add one third of water compared to the amount of non-polar with dissolved dmt fb.

Anyway, you should get rid of the emulsion as some dmt is trapped within it. You can heat it as you wish, it can even boil (this sometimes helps), if lower temperature won't help. While heated, you can use ocassional careful moving/stirring or better some kind of vibrations (washer, attached mobile phone, ...). If not successfull, you can leave it somewhere for few days, this can help as well.
I wouldn't use NaCl, as it might push salted dmt out of the water.
If you have problem with salting by vinegar, you can try another acid.
 
Yes you suggested 1/3 water but i wanted to experiment with 500mg dmt only if something goes wrong i dont loose much of it so i used only 20ml of nps and 1/3 of that is too small amount to work with. this is why i added more water. i think it should be no problem. also i made the HP 2,9 so there is more vinegar as well...

Interesting when the liquid is hot the layers are more clear and the white layer is very thin too but if the liquid cools down the layers get more turbid (much less clear) and the white layer thickens. Its strange because i think once the emulsion is broken then it cannot grow again.

okay, i will try as you suggested.
Thank you for your time :)
 

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