Striving to get pure white spice

[MachineElf88]

Hey guys, I wonder if anyone can help me here. My spice always comes out yellow. I do STB or a hybrid and it's all good. The yellow works just fine.

But.....

I just want to get it to pure white just to see what it's like. I've never had it and I've read it's much smoother to vape. Also there's just that striving for perfection in a Walter White kind of way

In my latest extraction I did my usual STB then did a mini a/b on the result. Got nice yellow crystals.

I'm now trying to wash those yellow crystals. So I dissolved in boiling solvent and then added a pinch of sodium carb to some luke warm water. I mixed the two and then separated. I repeated 3 times and now I've just finished my 3rd wash and each time I can see the impurities floating around in the water but my solvent is still bright yellow.

So my questions are -

1. Should my solvent be clear once all the impurities have been removed or is what I've done enough?

2. Is there anything else I can do besides a re X with Heptane afterwards if it's still yellow?

3. Am I trying to get something that isn't possible to get because of my source material? Mimosa hostillis

ps. I know I can probably get a white product easily with an A/B but I just hate dealing with the cooks and filtering.

Thanks

 

[1ce]

Pull freebase with whatever solvent you have, wash it with water to remove basic material, clean it up with a pinch of activated carbon. Filter the carbon out very thoroughly, rinse filter papers with pure solvent. Do a base->acid, was with cold non polar, do an acid->base, extract with heptane, crystallize slowly.

Walter White would have clear rhomboid crystals, not white powder

 

[MachineElf88]

Ok so just to be clear -

1. Pull freebase
2. Wash with water
3. Clean with acitvated carbon
4. Filter carbon out
5. Base to Acid
6. Wash with solvent
7. Acid to base
8. Extract with Heptane

A few questions -

I've Never used activated charcoal before. So I just add powdered charcoal to the solvent, mix and then filter it out with coffee filter paper. Then just put pure solvent through the paper to get any spice trapped in the paper. Is this all correct?

I read that carbon can really eat into your yield, is that just the price you have to pay for pure spice?

 

[1ce]

Ok so just to be clear -

1. Pull freebase
2. Wash with water
3. Clean with acitvated carbon
4. Filter carbon out
5. Base to Acid
6. Wash with solvent
7. Acid to base
8. Extract with Heptane

A few questions -

I've Never used activated charcoal before. So I just add powdered charcoal to the solvent, mix and then filter it out with coffee filter paper. Then just put pure solvent through the paper to get any spice trapped in the paper. Is this all correct?

I read that carbon can really eat into your yield, is that just the price you have to pay for pure spice?

Yes, there is a price to pay for a pure product. Just use a pinch and swirl from time to time, the solvent will clear up tremendously. I've always used carbon and I have not observes a noticeable loss in my yields. If you're using DCM/TCM as your solvent do not wash your acidic phase, since DMT salts may be soluble in chlorinated hydrocarbons. Allow heptane to evaporate slowly at room temperature. Use aluminum foil, poke a few small holes in it for a lid. Let it evaporate to half or 1/3 volume. Move this to the refridgerator for a few hours, finally the freezer.

For your crystallizing dish, rinse it with water, and clean it with acetone and paper towels. Allow it to evaporate to dryness. Acetone is a glass cleaning champion, but be aware that it attacks plastic. A crystallization is similar to a distillation as a purification step. It takes time. Do not allow the solvent to evaporate completely (use a lid) as impurities will remain in the solvent, and will layer your crystals if you allow them to fall out of the solvent. The theory is to allow the purest fraction of DMT to fall out, not ALL of it. Simply reuse your solvent to get some of the left-overs out.

 

[Orion]

Mini A/B.

 

[concombres]

You could go the fasa route then wash fumarates with dry acetone, base, water wash, re-convert back to fumarate & repeat until it's white. But ice's method is much quicker & has less potential for yeild loss that would need to be recovered.

Just don't use craploads of activated carbon or you'll lose craploads of yeild.

 

[Nereus]

Extract cold!

Sure yield will be affected but will pull less oils and just a simple re-x will result in white fluffy goodness.

 

[MachineElf88]

Thanks for the replies. A lot of that I was already doing.

I will use activated charcoal on my next one.

 

[entheogenic-gnosis]

Have you read about DMT polymorphism?

http://www.sciencedirect.com/science/article/pii/S0026265X13000544

Read the section on the color of the DMT crystals, it may help clear things up.

-EG

 

[1ce]

Have you read about DMT polymorphism?

http://www.sciencedirect.com/science/article/pii/S0026265X13000544

Read the section on the color of the DMT crystals, it may help clear things up.

-EG

Yeah, there was SPECULATION that the polymorph MIGHT affect crystal coloration. I've read speculation that the polymorph only exists in a liquid and vapor form.

With that out of the way I have noticed 2 congruent, repeatable instances. I present: Yellow DMT is known to have contamination. Ask anyone utwith yellow butter crystals and they'll probably admit an oily batch. But there's just one thing, one thing that irks me the most over this whole polymorph speculation. Why is it these urine colored crystals magically stop being yellow when purification steps are added in? Why is it they suddenly disappear?

Is the polymorph insoluble in heptane? I don't think this is the case.

Just clearing that up,
1ce

 

[AcaciaConfusedYah]

Yellow isn't 'bad.' It's just not white. I've had some seriously powerful trips on yellow crystal. Maybe more powerful than some of the clear shards that I've yielded.

However, I empathize with you for wanting to pull clear or white shards. It's more of a personal sense of accomplishment than the quest for a "better" or "cleaner" trip.

it's kinda funny.... only recently have I begun to be more concerned with white spice. BUT I have not really been smoking much during the past 6 months. SO...for looking at - I conclude that white spice is the best! But for smoking, it all works

 

[entheogenic-gnosis]

Thus far I've never heard anyone contest DMT polymorphism, and I'm actually kind of glad, if you can provide evidence as to why DMT polymorphism is not a valid explanation for multiple melting points and colors of DMT I would gladly change my views.

When presented with new evidence any scientist would evaluate said evidence and alter his views accordingly.

DMT polymorphism seems to be a logical explanation as to why pure DMT cam be yellow or have variable melting points.

I should also point out that lye is white so lack of color doesnt guarantee a pure product either.

I didn't mean to hit a sensitive nerve with you or anything, but according to the evidence that I have been presented with this seems to be the case. If you can provide evidence contrary to this I would be happy to go over it, and if the evidence points to DMT polymorphism being such wild speculation as you say, I'll gladly change my position on the topic.

-EG

 

[1ce]

Thus far I've never heard anyone contest DMT polymorphism, and I'm actually kind of glad, if you can provide evidence as to why DMT polymorphism is not a valid explanation for multiple melting points and colors of DMT I would gladly change my views.

When presented with new evidence any scientist would evaluate said evidence and alter his views accordingly.

DMT polymorphism seems to be a logical explanation as to why pure DMT cam be yellow or have variable melting points.

I should also point out that lye is white so lack of color doesnt guarantee a pure product either.

I didn't mean to hit a sensitive nerve with you or anything, but according to the evidence that I have been presented with this seems to be the case. If you can provide evidence contrary to this I would be happy to go over it, and if the evidence points to DMT polymorphism being such wild speculation as you say, I'll gladly change my position on the topic.

-EG

I'm not contesting polymorphism, I'm contesting that polymorphism has anything to do with yielding yellow crystals. I've seen synthetic DMT exist as yellow goo/crystals where NMT was the culprit. NMT affliction exists no matter where the entheogen came from. TiHKAL describes reacting NMT with acetic anhydride or benzoyl chloride to remove NMT. Column chromatography is an option as well.

Sofar the only evidence I've seen regarding crystal coloration is that an excess of NMT/DMT-oxide results in the discoloration of the target product.

You haven't struck a nerve bud I see alot of people holding the polymorph responsible for yellow crystals. Yet the only article that can be cited uses the word "might". Playing devil's advocate there is no evidence at this time to authoratively state the polymorph has no effect over refraction of light within the crystaline structure.

There is one thing I can offer as fact, and that is I can continuously obtain yellow urchin crystals, or transparent needlepoints. Each by following the same repeatable proceedure each and every single time.

 

[Orion]

EDIT: found the other article and attached...

Why is it these urine colored crystals magically stop being yellow when purification steps are added in? Why is it they suddenly disappear?

I have never seen clear white spice become yellow in any simple alkane solvent, though I have observed every shape under the sun forming, and not a single one was any other colour than the starting colour. I've also never seen one single example of this happening from anyone else on the forum. This doesn't include evapping solvent down onto crystals that formed at room temp (obviously the gunk in the solvent becomes more visible as the solvent evaps and discolors the alks).

I'll attach the paper that mentions DMT Hydrobromide being 'transparent light yellow prisms'. I've also attached the freebase DMT polymorphism vs colour thing...

'DMT samples were
prepared following extraction from Mimosa tenuiflora inner barks or by laboratory synthesis and then its crystals were recrystallized from solutions of the alkaloid using either hexane or acetonitrile. Irrespective of source, crystals originating from synthesis were predominantly white crystals obtained using crystallization from hexane, whereas yellow samples following recrystallization with acetonitrile. Irrespective of source or solvent, two polymorphs appeared to exist with melting points, determined by DSC, of 57°C to 58 °C for Form I and 45 °C to 46 °C for Form II. Estimates for their enthalpies were 91.9 ± 2.4 J g−1 for Form I and 98.3 ± 2.8 J g−1 for Form II. Form II converted to Form I during DSC; conversion was thus prevented by fast scanning rates of 100 °C min−1. A transition temperature (Tg) in the range −21 °C (2 °C min−1) to −13 °C (100 °C min−1) was determined depending on DSC scanning rate. Its closeness to the melting point indicates a tendency of Form II to convert to Form I on storage, a phenomenon that was also facilitated by grinding. This study indicates that the presence of differently colored DMT free base crystals obtained from recrystallization might also point towards the existence of polymorphs rather than just the presence of impurities.'


All this seems to really say is that acetonitrile gives you yellow spice if you try to recrystalize with it, and that these polymorphs are present in whatever solvent you use. It mentions DMT becoming yellow over time, something we all knew anyway. This piece of info does not even seem to suggest that the solvents themselves affect polymorphism. All it seems to be saying is that one polymorph can become another. It says it suggests that the presence of colour could be due to polymorphism, but the only example it gives of a colour change was in a different solvent which was always yellow, even though it too had different polymorphs just like hexane did. If it has the same polymorphs but both are yellow, and the other solvent gave different polymorphs and they were clear, then how does this suggest polymorphs affect colour? It sounds like it's saying the exact opposite. And which spice did they re-x in acetonitrile, the extracted stuff or the synthetic stuff or both ? What colour was each to begin with ?

I dunno, this seems flaky at best, but that's just me. Anyone wanna try getting some glassy super pure white spice and re-x in acetonitrile and see if it gives yellow crystals?

 

[1ce]

EDIT: found the other article and attached...

Why is it these urine colored crystals magically stop being yellow when purification steps are added in? Why is it they suddenly disappear?

I have never seen clear white spice become yellow in any simple alkane solvent, though I have observed every shape under the sun forming, and not a single one was any other colour than the starting colour. I've also never seen one single example of this happening from anyone else on the forum. This doesn't include evapping solvent down onto crystals that formed at room temp (obviously the gunk in the solvent becomes more visible as the solvent evaps and discolors the alks).

I'll attach the paper that mentions DMT Hydrobromide being 'transparent light yellow prisms'. I've also attached the freebase DMT polymorphism vs colour thing...

'DMT samples were
prepared following extraction from Mimosa tenuiflora inner barks or by laboratory synthesis and then its crystals were recrystallized from solutions of the alkaloid using either hexane or acetonitrile. Irrespective of source, crystals originating from synthesis were predominantly white crystals obtained using crystallization from hexane, whereas yellow samples following recrystallization with acetonitrile. Irrespective of source or solvent, two polymorphs appeared to exist with melting points, determined by DSC, of 57°C to 58 °C for Form I and 45 °C to 46 °C for Form II. Estimates for their enthalpies were 91.9 ± 2.4 J g−1 for Form I and 98.3 ± 2.8 J g−1 for Form II. Form II converted to Form I during DSC; conversion was thus prevented by fast scanning rates of 100 °C min−1. A transition temperature (Tg) in the range −21 °C (2 °C min−1) to −13 °C (100 °C min−1) was determined depending on DSC scanning rate. Its closeness to the melting point indicates a tendency of Form II to convert to Form I on storage, a phenomenon that was also facilitated by grinding. This study indicates that the presence of differently colored DMT free base crystals obtained from recrystallization might also point towards the existence of polymorphs rather than just the presence of impurities.'


All this seems to really say is that acetonitrile gives you yellow spice if you try to recrystalize with it, and that these polymorphs are present in whatever solvent you use. It mentions DMT becoming yellow over time, something we all knew anyway. This piece of info does not even seem to suggest that the solvents themselves affect polymorphism. All it seems to be saying is that one polymorph can become another. It says it suggests that the presence of colour could be due to polymorphism, but the only example it gives of a colour change was in a different solvent which was always yellow, even though it too had different polymorphs just like hexane did. If it has the same polymorphs but both are yellow, and the other solvent gave different polymorphs and they were clear, then how does this suggest polymorphs affect colour? It sounds like it's saying the exact opposite. And which spice did they re-x in acetonitrile, the extracted stuff or the synthetic stuff or both ? What colour was each to begin with ?

I dunno, this seems flaky at best, but that's just me. Anyone wanna try getting some glassy super pure white spice and re-x in acetonitrile and see if it gives yellow crystals?

Thankyou, that's what I've been trying to get across. That while there exists a polymorphic variant there's nothing to indicate it has anything to do with color. They didn't specify method of crystallization. They also couldn't distinguish the source of the sample DMT, which can be problematic since synthetic DMT can be extracted from the reaction solution with an impurity inseparable with crystallization. These impurities have a significantly higher boiling/melting point than DMT.

The article also mentions that the yellow polymorph reverts to the form of the white polymorph under storage but doesn't detail anything beyond that. One could take from this that again the polymorph only exists as a liquid or vapor but again that's speculation.

People are taking too much from these detail lacking reports as an absolute fact. Sofar all we know is there is a polymorph, and nothing else.

 

[1ce]

Also with such a miniscule difference in mp between 'form I' and 'form II', could partial pressure play an influential role in the mp/bp of these compounds? I don't see any spectra/chromatagrams in any of these studies to provide a composition list of what was found in the DMT.

My logic is: We have known impurities that influence crystal coloration and can be hard to separate. We've also observed different melting/boiling points of DMT with no real testing included to determine makeup/purity. Yet through some form of mental gymnastics we're assuming that a wild polymorph suddenly appeared and that has everything to do with crystal coloration and operator error has no role to play. (said operator has no clue where the dmt even came from in some cases, so isolation is moot)

Perhaps there is some very thorough confirmed scientific data I'm just not seeing. I believe myself to be "on mark" however.

 

[Orion]

Exactly 1ce, and even if someone gets white spice to become yellow (pics please), it still does not prove it has anything to do with polymorphism since all other solvents can give different polymorphs, and hexane and acetonitrile give the same polymorphs. I am interested to see the colour change in acetonitrile though, but I guess nobody is willing to turn their lovely glassy spice yellow again since it proves nothing.

 

[1ce]

Exactly 1ce, and even if someone gets white spice to become yellow (pics please), it still does not prove it has anything to do with polymorphism since all other solvents can give different polymorphs, and hexane and acetonitrile give the same polymorphs. I am interested to see the colour change in acetonitrile though, but I guess nobody is willing to turn their lovely glassy spice yellow again since it proves nothing.

On one note I'm lenient toward white/clear spice being 'the more pure' spice. Since we can in a reasonable fashion conclude that colored impurities such as oxide/nmt aren't present. NaOH shouldn't be a concern with proper cleanup toward the end of the extraction. (NaOH most likely won't be white since it'll be accompanied with black basic soup, yet people never fail to amaze..)

I personally transparent needlepoint shards. Not the urchin like clusters, but individual needles.

 

[DMTripper]

I used to get pure white spice. Then I had a bag of MHRB for about 2 years without extracting and when I started to use it again I always got yellow spice. I think it just got oxidised. I tried many times to get white again but never managed.

But now I don't care anymore. The yellow works just fine

 

[1ce]

I used to get pure white spice. Then I had a bag of MHRB for about 2 years without extracting and when I started to use it again I always got yellow spice. I think it just got oxidised. I tried many times to get white again but never managed.

But now I don't care anymore. The yellow works just fine

Why not oxidize your entire yield, then reduce it back.