recrystallization will not remove yellow

[concombres]

I had ~2g of yellow spice. Recrystallized last night & the yellow will not go away.
i dissolved in ~90ml hot, fresh naphtha, some goo fell out & then i freeze precipped only to get spice that was just as yellow.

Tried again today & have the same problem. When the spice is dissloved into the solvent, the solvent turns yellow & any goo dissolves in when stirred.

Right now i have 1.5g dissolved in 80ml solvent sitting in a heat bath returning to room temp but the solvent is showing no signs of color loss or impurities precipitating.

 

[AcaciaConfusedYah]

I had the same situation as you.... could not get rid of the yellow.

I finally accomplished this by doing a mini a/b after all the first pulls were collected.

Have you seen earthwalker's write up about adding a mini a/b to the end of Cyb's hybrid salt tek? It works, and it finally left me with pretty, fluffy, white crystals.


Dissolve all your yellow spice into some NPS. Bring ~400ml of distilled water to a ph of about 2.0. I use citric acid, other people use vinegar. Add the yellow nps to the acidic water.

The acidic solution will convert the molecule back into the salt form, which is not soluble in NPS, however the plant fats and oils are sill in the NPS.

I shook it up vigorously for about an hour or so before decanting the NPS that contained the yellow plant fats. I saved the used NPS to clean and use again on a later date. It can be reused or thrown away - your choice.

Re basify the solution by mixing 50g of NaOH to 200ml of cool water, and then add to the 400ml of acidic solution that contains the molecule in its salt form. The soliution will turn whitish. Do a few pulls with NPS of choice, and then continue your normal multidimensional television program.

 

[Entheogenerator]

Who ever said that it would? Read the recrystallization wiki page, particularly section 1.4.

 

[concombres]

:shock: Wow ive read that before a few times & never noticed the coloration part.

Ill keep the yellow this time & see how i like it. Next extraction ill work on a more white product & compare.

Mini a/b seems like it will cause alot less loss in product than a sodium carnonate or activated charcoal wash. Ill try that & see if i cant get nice white spice & grow some clear shards via slow room temp. Evap in a covered wine glass with some holes poked in the foil

 

[Entheogenerator]

Sodium carbonate washes have never removed coloration for me. The only method I have found to be effective is the activated charcoal method from the wiki.

 

[desal]

I had ~2g of yellow spice. Recrystallized last night & the yellow will not go away.
i dissolved in ~90ml hot, fresh naphtha, some goo fell out & then i freeze precipped only to get spice that was just as yellow.

Tried again today & have the same problem. When the spice is dissloved into the solvent, the solvent turns yellow & any goo dissolves in when stirred.

Right now i have 1.5g dissolved in 80ml solvent sitting in a heat bath returning to room temp but the solvent is showing no signs of color loss or impurities precipitating.

How hot is the naphtha? If the naphtha is too hot, it will dissolve the impurities along with the spice. I was having the same problem as yourself, I would end up with just as yellow spice. I thought i wanted to dissolve the spice into the hot solvent, but that just dissolved the impurities too. but I have fixed it now. i just did this earlier today so it's fresh in my mind, i was working with 1.3G of yellow dmt. I have a hot plate, so I set it to 50 degrees celcius, and warmed up some water. I put 40mL of fresh naphtha in a beaker and placed the beaker in the water to warm up. I put the 1.3G of yellow dmt in a separate jar, and did NOT put this jar in the warm water. ** this is key, if you put the spice into a too hot heat bath, the impurities will melt with it. so it is best to just warm up the naphtha to 50C and work it into the spice yourself, without melting the spice**

after a couple minutes, i touched my finger to the naphtha and it was warm, not hot (you dont want it to be hot, just warm). I took a pipette, and sucked up some of the naphtha, not all of it, and, holding the jar at an angle so that all of the spice was in a corner, I slowly dripped the naphtha in the spice jar until it covered the 1.3G, making sure to hold it at an angle so that it was all contained in a corner rather than sitting flat, and then added a little bit more naphtha on top, so that a) i could see the naphtha over the spice and b) i could put my pipette in the naphtha and suck the naphtha up without pulling any spice into the pipette. note that this is only like 1/4 or 1/3 of the total naphtha i had warmed up, like 10 to 20 mL, it is best to work with small amounts rather than too much, in my experience.

from here, I swirled the naphtha around in the jar, but i noticed this would cause some of the spice to be stuck around the jar, so I sucked naphtha up and tilted the jar again, and then squirted naphtha around to get all the spice back into the corner. then I sucked up the naphtha, and squirted it into the spice to mix the goo around. i did this for a little bit, but made sure not to be overly aggressive, we want the naphtha to remain clear. the dmt immediately dissolves into the naphtha, so after a minute or so, I separated the naphtha into a separate pyrex dish. you can do this by first sucking up all the naphtha on top of the goo, then, because you have kept all the goo in one corner, you can roll the jar so any remaining naphtha rolls to the other side where the goo is not, and you can suck it up cleanly.

then, repeat with a little bit more warm, clear naphtha. keep sucking the naphtha up and squirting it back into the goo, keep mixing the goo around and then getting all the goo back into one pile, then while it is still clear, separate the naphtha into a separate dish and do it again and again. each time you do it, the goo will get smaller, but the naphtha will remain clear. you can be sure that there is dmt in each batch of clear naphtha by blowing into the naphtha for a couple seconds until you see clouds appear.

keep doing this, little bit of naphtha at a time, until the goo pretty much disappears. eventually you will notice a glob of stuff which doesn't dissolve, and is probably mixed with hair, just pull this out with your finger or the eyedropper. i was only doing 1.3 grams, and had to add a little bit more naphtha to my beaker, and let that warm up for a couple minutes before using it to completely wash all the goo in the other jar. all this naphtha that you combine together in a separate jar or pyrex dish, you can freeze precipitate or evaporate. It should cloud up as soon as you put it onto a pyrex plate, or into another jar, and because you are using such a little amount of naphtha, you could set it under a fan and it will evaporate pretty much before your eyes. although, this might leave a very very light yellow tint to SOME of the crystals, which you can just wash again like this and get rid of. or you could freeze precip and probably bypass that yellow.


i ended up with 1.15 grams of shiny white crystal, although there was a very very light yellow tint to SOME of it, which I will wash out by doing this again.

if doing two grams, you will probably need more than 40mL, so you could start with 80mL warmed up in a beaker, just don't add all of it to your spice at once. (you could, but i have better luck doing it little by little. this way you don't use too much and it will evaporate quicker)

key points:

A) do not heat the naphtha up to more than 40 - 50C, I use 50C, but you may be able to do this with 40C.
B) do not melt the spice down, add the warm naphtha to the non melted spice,
C) Warm up all the naphtha at once, but only add 10 to 20mL at a time to the spice, just enough to cover the spice and some more on top so you can separate it from the spice easily, but not a whole bunch
D) swirl the naphtha around, use an eyedropper and suck the naphtha up and push the naphtha into the goo so that goo moves around, or physically move the goo back and forth with the eyedropper itself, but this might get goo stuck to the eyedropper, but keep the goo all together on one side of the jar, it is easier to work with in my opinion
E) ** this is the big one for me ** -- you want the naphtha to remain clear while this is happening, and it will unless you made it too hot... but while the naphtha is still clear, separate it into a different container and then repeat with another small amount of naphtha.

 

[desal]

I have tried multiple teks, using heat, not using heat, STB, A/B, hybrid, etc, but I found that with heat, anything over 40 to 50C is going to bring more impurities, more yellows, oranges, etc. and now that i've tried all of them, I am finding I actually get very nice white crystals with STB. the heat from the lye is all the heat you need. White crystals / goo, although after drying them out with a fan, and then scraping them, they turn a little yellow, but then the above re-crystallization method does bring them back to sparkling, shiny white. the whiter crystals you start out with, the less you need to re-x them.

I just did an excellent extraction with 100G shredded (practically powdered but not really) MHRB.

I put 100G MHRB in a 1L flask. Then I warmed up 200mL water to 50C and added 50G non-iodized salt, stirring until all the salt was dissolved. then I added the 200mL water to the flask.

Then I put 500mL water in a separate flask, and added 76 grams of lye to this water, put a stopper on the flask, and shook it up until it was all dissolved in the water (this does get hot and you want to be careful because the stopper will pop off with pressure, so hold a rag over the stopper and release the pressure slowly after shaking it)

then I added this 500mL water to the 1L flask with the MHRB and salt-water in it. and shook thoroughly. everything went black. usually here, teks will have you wait for awhile, but you dont need to, in fact, i find if you just go ahead and extract now, you can get some very white crystals and you can always leave the jar overnight and extract again the next day.

then I added 50mL of naphtha, and rolled, and turned, and swirled, and shifted end over end, and then shook it up a bunch, for at least 10 to 20 minutes or so (if you want to avoid emulsion, skip this shaking part, but I find that the emulsion separated pretty quickly) and allow to separate until there is a clear separation between the two. if you have emulsion, swirling the liquid will help it separate, and so will tapping the jar. (you could add more salt or more lye to the solution as well, but it should separate fairly quickly. a heat bath would also help separate it but will bring more impurities and this is what we are trying to avoid, so just be patient) mix it all up and let it separate three or four times, and then use a pipette to separate the naphtha into a separate container. when you get close to the lye-mimosa-water, leave the naphtha (we will get it on the last pull) and add 50mL more naphtha and repeat the shaking / separating process.

around the third pull [for me] the heat from the lye had pretty much cooled off, so I added another 100mL of water to a separate flask, and poured maybe .. 20 to 30G lye [ i didn't measure it, i just poured enough in to cause heat + saturation ] into the flask and shook it up, then added it to the 1L flask with the rest of the soup. this warmed up the soup and added some more water / lye for the naphtha to move through.

after this, i did two more 50mL pulls, and am now leaving the jar to soak for 24 to 48 hours before pulling some more.

when i get to the very bottom of the last pull, where the naphtha meets the soup, it becomes difficult to pull the naphtha out without getting mimosa into the mix, so instead of pouring directly into the container i have been using, I pull out a graduated cylinder (any container which is tall and skinny will work) and i put the last of the naphtha in here, this way i dont have to worry about accidentally pulling some mimosa mix too, because I can let this settle out and then move it to the jar with the rest of the naphtha, leaving any mimosa behind in this intermediate container.

each pull, i combined together, and then placed under a fan for a little while to reduce the volume a little, for the purpose of increasing the saturation of DMT in the liquid. you will see the liquid start to get very cloudy. if you leave it long enough, crystals will even start forming on the sides where the solution has evaporated at. once it gets cloudy, i cover it and put it into the freezer overnight.

the next day, bring a jar and an eyedropper/pipette, and open up the freezer, uncover the lid (or remove the foil/saran wrap, whatever cover you used) and tilt the jar so that all the naphtha runs to one corner, and use the eyedropper/pipette to suck it up and put it into the jar (or just tilt it and pour it into the jar, but if there are any crystals floating around, you will want to pour through a coffee filter to catch them, or just use a pipette so they will stick to the jar when the naphtha level gets low) then, put the jar upside down in the fridge for awhile, so that any naphtha will a) roll away from the crystals and b) the glass will warm up a little bit without getting too much condensation on it.

you can skip the fridge part and just pull the dish out and place it in front of a fan, on high, until dry, but ive noticed that the sudden change in temperature causes a bunch of condensation, and the water can affect the crystals. let them dry, scrape them up, and put them onto different plate to dry out further. after this, is when I combine them into a jar and do a re-crystallization as described above. i always do at least one re-x just to be sure that the spice is clean, and then you can do more if you want.

 

[benzyme]

+1 on the AC method, it is great for decolorizing when tannins are present.

whatever method you choose, consider purging the storage vessel with some inert gas if you plan to store your dmt as a free base, or it will get a yellowish tint over time. this property is inherent to simple tryptamines, and tryptamine itself.

 

[1ce]

+1 on the AC method, it is great for decolorizing when tannins are present.

whatever method you choose, consider purging the storage vessel with some inert gas if you plan to store your dmt as a free base, or it will get a yellowish tint over time. this property is inherent to simple tryptamines, and tryptamine itself.

I'm with you here, I want to post a guide within the next few days to help people START with a higher purity product so they don't have to kill their yield recrystalizing too much.

I'd also like to say that washing your solvent with distilled water a couple of times works well too. Helps removed alot of that lye based contamination as well. After I reduce my volume I'll clean up with AC and filter it off.

 

[Earthwalker]

I'd also like to say that washing your solvent with distilled water a couple of times works well too. Helps removed alot of that lye based contamination

I see you repeating this claim about lye ridden DMT over an over and i don't no how careful you are at removing the nps from you're basic soup during the extraction because that is the only way lye can end up in the end product as lye isn't soluble in naphtha ! Am I correct in saying this ??

 

[SnozzleBerry]

I'm with you here, I want to post a guide within the next few days to help people START with a higher purity product so they don't have to kill their yield recrystalizing too much.

By all means, feel free to share...but it's not really that big of a deal, imo. As burnt's analysis showed, even dark red DMT is still like ~95% DMT. So talking about "purity" is kind of unfounded...aesthetic seems a more apt term given the percent purity we've seen in the past (to say nothing of the polymorphic qualities of DMT).

 

[○]

Yeah, lye contamination only shows up if your sloppy with pulling the NPS.

And yeah, the whole purity - yellow/white/orangeyellow DMT thing, as snozz said - aesthetic value is more play at here then the whole 'purity' thing.

Extract DMT (if there's no lye contam) - smoke DMT.

 

[starway6]

Agreed..but at the celular level.. no one knows what impuritys do to our bodys over time..
May not be any worse than smoking a cigarette twice a week.?
The human biological celular code is where the risk lies....and having a more pure product is not a bad idea.. ..i think..

 

[AcaciaConfusedYah]

When people brew tea, they drink all the impurities and then some. I wouldn't worry too much about the health side of impurities from the plant.

 

[1ce]

I'm with you here, I want to post a guide within the next few days to help people START with a higher purity product so they don't have to kill their yield recrystalizing too much.

By all means, feel free to share...but it's not really that big of a deal, imo. As burnt's analysis showed, even dark red DMT is still like ~95% DMT. So talking about "purity" is kind of unfounded...aesthetic seems a more apt term given the percent purity we've seen in the past (to say nothing of the polymorphic qualities of DMT).

Yeah but cleaner spice sure does taste alot better. I'll smoalk yellow spice any day. But I give my mates the cleanest spice I can achieve.

Also Snozz, I see alot of basic lab extraction techniques go completely ignored. They're time proven and taught in schools for a reason >.<

I agree, If my spice is a little yellow I'll keep it. But my spice is never yellow anymore that's just the thing. I focus on doing everything as correctly as possible the first time so product isn't lost cleaning it up later.

For me at least, it's been worth while =] And I hope my efforts help prevent some of the more repetitive questions I see.

Aestetically pleasing crystals aren't a bad thing either 8)

 

[The Traveler]

I'd also like to say that washing your solvent with distilled water a couple of times works well too. Helps removed alot of that lye based contamination as well. After I reduce my volume I'll clean up with AC and filter it off.

Be careful not to express your wording in such a way that people get the idea that coloration is only caused by lye contamination. People often judge too quickly and research too little to know that this is a false claim, so again please be careful how you express yourself here as to not cause confusion and possible misinformation.

For example, at times my spice extractions came out colored but even after multiple conversions to DMT-fumarate and back did it not remove any of that coloration. Therefore it ruled out that in this case the coloration was due to lye contamination.


Kind regards,

The Traveler

 

[1ce]

True, I did not mean it that way. I'm working on a pictorial as I post this. In experience I find a couple things almost always lead to discoloration.

Reusing my solvent. I am in NO WAY suggesting this is bad, you just have alot more tannins and other alks as salutes. These probably just fall out as you precip.

Leaving my spice sitting out in the open. I am completely guilty of this. I left a dish of spice out for a few days and my whiter than snow spice now has alot of yellow. This is fine, it vapes well, tastes well, it's just a little discolored.

My reference to lye based impurities falls with the implication of using naptha, or a top separating solvent. The naptha generally remains on top so as one would wash with distilled water to remove any water soluble crud it would wash out any basified material at the bottom.

I'd be very apriciative if you and some of the mods critisize my pictorial because I value your imput.

Also I don't think oxide conversions are all that useful. Washing almost always goes along side extractions, why exclude it? Between this and an A/C wash my spice looses almost all of its color.

You are absolutely right though traveler. Colorization absolutely does not mean harmful contamination and thank you bringing this up. I did not intentionally mean to propagate this and I will try to stay vigilant of it.

 

[starway6]

I know most people smoke crystals or goo..or changa.ect...
I simply cause an oversaturation pour off exess napatha in clean jar and quickly fan dry the crystals till they are dry as powder..
Then i desolve my crystals in grain alcohol for easy storage in almost any temperature for months if needed..
Then the convieniance of putting 10...15...0r 30 drops of my tinture in a small wad of volcano wet pad is super easy!
I always let the porus wet pad dry for atleast 2 or 3 hours to asure that the tinture is compleatly void of grain alcohol and any trace amounts of napatha!
Works well for me..but if anyone can think of a better safer way to improve on this method..
Please let me know...
Im surprised not hearing of more people using the DMT tinture method!?

below are photos..

 

[1ce]

I know most people smoke crystals or goo..or changa.ect...
I simply cause an oversaturation pour off exess napatha in clean jar and quickly fan dry the crystals till they are dry as powder..
Then i desolve my crystals in grain alcohol for easy storage in almost any temperature for months if needed..
Then the convieniance of putting 10...15...0r 30 drops of my tinture in a small wad of volcano wet pad is super easy!
I always let the porus wet pad dry for atleast 2 or 3 hours to asure that the tinture is compleatly void of grain alcohol and any trace amounts of napatha!
Works well for me..but if anyone can think of a better safer way to improve on this method..
Please let me know...
Im surprised not hearing of more people using the DMT tinture method!?

below are photos..

Your post really piques my interest! I've often wondered about using a binary solvent like ethanol/water because DMT has crap solubility in water. One should in theory be able to dissolve their spice in an azeotropic sokution and store. Then simply dilute it with distilled water and precip at lower temps.

I would love to try this soon enough and share what I find with the community.

 

[starway6]

I know most people smoke crystals or goo..or changa.ect...
I simply cause an oversaturation pour off exess napatha in clean jar and quickly fan dry the crystals till they are dry as powder..
Then i desolve my crystals in grain alcohol for easy storage in almost any temperature for months if needed..
Then the convieniance of putting 10...15...0r 30 drops of my tinture in a small wad of volcano wet pad is super easy!
I always let the porus wet pad dry for atleast 2 or 3 hours to asure that the tinture is compleatly void of grain alcohol and any trace amounts of napatha!
Works well for me..but if anyone can think of a better safer way to improve on this method..
Please let me know...
Im surprised not hearing of more people using the DMT tinture method!?

below are photos..

Your post really piques my interest! I've often wondered about using a binary solvent like ethanol/water because DMT has crap solubility in water. One should in theory be able to dissolve their spice in an azeotropic sokution and store. Then simply dilute it with distilled water and precip at lower temps.

I would love to try this soon enough and share what I find with the community.

As far as i can tell it stores in grain alcohol great..no need to worry about crystals melting if frige stops working..
It seems to stay stable in alkmost any temperature and as long as one alows the tinture to compleatly dry it should be clean and free of any trace napatha and aplying drops to some fine mesh pad is easy and drys quickly because the pad [although densly compressed]..alows good ventilation to evaporate the alcohol and any trace napatha...
I vape this way through a water pipe incase ..although doubtful that any trace lye got through].... the water should trap it preventing me from inhaling any..
Im still trying to send my photos above.. but im using google chrome and the procedure to send photos is a little diferent than im used to..ill keep trying...
There was someone on the forum that is test storing some alcohol dmt tinture for a year to see if it caused any degrading of the molecule..
[Ethenator] I think was doing this test?