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Dmt eveporating when evaporating naphtha? Options
 
chinkof
#1 Posted : 1/22/2020 9:20:09 AM

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Hi.

So I've been trying multiple methods to try and get the best possible, clean yield.

I've tried A/B and straight to base.

I might have done something wrong with the straight to base extraction. States below is the way I've done this:

1. Powdered 252grams of MHRB, fine powder with tiny fibers in it.
2. Measured 15ml of demi water per gram of root bark.
3. Mixed in the semi water 252 grams of natrium hydroxide grains into the water, shaked this until it was an clear solution. PH was around 11-13, pH papers weren't very clear.
4. Added the MHRB to the base solution. Stirred and shaken this until it was one fluid.
5. Heated this fluid on low heat for around an hour, exact themp isn't measured.
6. Added 200ml of warm naphtha to this fluid and shaked it for a couple of minhtes
7. Shake 3-4 times and seperated until the first pull, this was around 24 hours after the naptha was added. This naphtha was two times washed with demi water. After that it was poured in a glass oven tray, and put into a freezer for around 48hours. This was then filtert through a paper filter. The oven tray then placed upside down on another oven tray and placed again in the freezer to let the naphtha completely out of the tray. This resulted in a end result of around 0,7 grams of pure and white Cristal.
8. New naphtha was added (warm) and shaken 10 times during 48 hours. This resulted in a cloudy brown naphtha layer. After some research I did in total 4 soda washes for the naphtha, this resulted in about 0,1 grams.
9. New naptha was added and shaken 20 times during 5 days. Another pull was done the same way as above.

Now I have a couple of questions that I got from this and other test I tried.
- When I got a pull of naphtha (cleaned 2-3times with water) I tried to vaporize it down to 3/5 of the starting amount with some really low heat(pot put into some hot water) . Every time I try this I seem to lose a lot of yield...
- With the soda wash I seem to have lost almost all the DMT, only 0,1 grams on the second pull, with the first one having 0,7 grams.
- I only got miniscule powder, no big crystals. Of course this has to do with the way I let the Cristal form (best way is to redissolve the current dmt into naphtha and then let it vaporize at room temp. At least for what I've read). But because I lose quite a lot in the washes or when I try to vaporize the naphtha I am scared that I will lose a lot/ all of it when I redissolve it and let it vaporize on room temp.



I've looked through all the teks, but couldn't find something I've done directly wrong (maybe I have over looked some thing?). Also I sketched all the steps I took globally.

Could you help me with this problem/low yield? Because (theoretical) I should get around 1.4 grams, but at the moment I have only half of that...


Thanks in advance

Chinkof
 

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endlessness
#2 Posted : 1/22/2020 12:22:32 PM

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DMT def doesnt evaporate with naphtha like that.

The possibility I see is that either your mimosa is low yielding to begin with, or that your naphtha isnt saturated enough so you need to pre-evap even more before putting in the freezer.

What do you do with the naphtha pulls after getting the crystals out, are you reusing it? You should otherwise at least, re-evap it down to very small amount again and then stick in the freezer again.
 
CosmicGigglez
#3 Posted : 1/22/2020 7:05:39 PM
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endlessness wrote:
DMT def doesnt evaporate with naphtha like that.

The possibility I see is that either your mimosa is low yielding to begin with, or that your naphtha isnt saturated enough so you need to pre-evap even more before putting in the freezer.

What do you do with the naphtha pulls after getting the crystals out, are you reusing it? You should otherwise at least, re-evap it down to very small amount again and then stick in the freezer again.
indubitably!
 
downwardsfromzero
#4 Posted : 1/23/2020 10:31:44 PM

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chinkof wrote:
Because (theoretical) I should get around 1.4 grams
1.4 grams from 258 grams of bark is a pretty poor yield, even. All those water/carbonate washes can't be helping. With decent bark (and technique...?) you could be getting about 5 grams.

Also, the naphtha pulls are far too long. They should only be as long as it takes to mix, then separate, mix, then separate (a few times) before syphoning off the naphtha. The 48 hour soak would be for the mix of the bark with the base, so that the woody material breaks down - although there's no harm in mixing in the first batch of naphtha at the start, I suppose. Saves 20 mins on the first pull. Maybe.

You would have done well to do 5 separate 50 gram extractions. For one thing, the amounts are a lot easier to handle.

Oh, and DMT co-distils with heavy naphtha at 140°C but hardly at all at room temperature.
Ora, lege, lege, lege, relege et labora

“To be GOVERNED is to be watched, inspected, spied upon, directed, law-driven, numbered, regulated, enrolled, indoctrinated, preached at, controlled, checked, estimated, valued, censured, commanded, by creatures who have neither the right nor the wisdom nor the virtue to do so. To be GOVERNED is to be at every operation, at every transaction noted, registered, counted, taxed, stamped, measured, numbered, assessed, licensed, authorized, admonished, prevented, forbidden, reformed, corrected, punished. It is, under pretext of public utility, and in the name of the general interest, to be place under contribution, drilled, fleeced, exploited, monopolized, extorted from, squeezed, hoaxed, robbed; then, at the slightest resistance, the first word of complaint, to be repressed, fined, vilified, harassed, hunted down, abused, clubbed, disarmed, bound, choked, imprisoned, judged, condemned, shot, deported, sacrificed, sold, betrayed; and to crown all, mocked, ridiculed, derided, outraged, dishonored. That is government; that is its justice; that is its morality."
― Pierre-Joseph Proudhon
 
chinkof
#5 Posted : 1/27/2020 3:38:02 PM

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CosmicGigglez wrote:
endlessness wrote:
DMT def doesnt evaporate with naphtha like that.

The possibility I see is that either your mimosa is low yielding to begin with, or that your naphtha isnt saturated enough so you need to pre-evap even more before putting in the freezer.

What do you do with the naphtha pulls after getting the crystals out, are you reusing it? You should otherwise at least, re-evap it down to very small amount again and then stick in the freezer again.
indubitably!


Thank you for your reply! I am sorry for my delayed reply Sad

I've got 1,7grams out of the 252 grams so far, I did try to evaporate the Naptha down to 1/5th of the starting amount, this gave me some yield indeed!

I got around 1.7grams, after 2 water washes I want to try and get some really big and white Cristals out of it (just to see how far we can go, I like to experiment with these thingsSmile. For what I've read about getting big crystals I need to get as pure as possible dmt, so it will cristalise better. Would you recommend a active coal wash with this? And then to let it evap at room temp in a wine glass?

Thanks again!


 
chinkof
#6 Posted : 1/27/2020 3:53:43 PM

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downwardsfromzero wrote:
chinkof wrote:
Because (theoretical) I should get around 1.4 grams
1.4 grams from 258 grams of bark is a pretty poor yield, even. All those water/carbonate washes can't be helping. With decent bark (and technique...?) you could be getting about 5 grams.

Also, the naphtha pulls are far too long. They should only be as long as it takes to mix, then separate, mix, then separate (a few times) before syphoning off the naphtha. The 48 hour soak would be for the mix of the bark with the base, so that the woody material breaks down - although there's no harm in mixing in the first batch of naphtha at the start, I suppose. Saves 20 mins on the first pull. Maybe.

You would have done well to do 5 separate 50 gram extractions. For one thing, the amounts are a lot easier to handle.

Oh, and DMT co-distils with heavy naphtha at 140°C but hardly at all at room temperature.


Thanks for your reply!! Sorry for my delayed one!

For what I've read MHRB contains about 0,57% of DMT, the inner root contains about 2%. Maybe I got it wrong, but when I try to do the math it should end with 1.4grams of pure DMT?

So for what I should've done is to firstly add the MHRB, and after I added the MHRB I should let it sit for 48hours, and shake it in those 48hours a couple of times. After the 48hours I should add some warm Naptha, shake it once, and then do it multiple times in a row before I take the naphtha off for cristalisation? The problem I got with this is that the naptha took a few times a bit longer before it completely seperates. And for what I've read in teks is to leave it a bit longer.

I totally agree that all those washes aren't helping at all. But an emulsion was formed so I had no choice to do those washes. Would you recommend to do only one demi water wash before cristalisation?

Wouldn't it be better if you shake the naphtha multiple times, so it can extract more dmt? Because more time will give the naphtha more chance to attract the dmt right? (could be me thinking like an idiot, but my thought about this is like a tea bag, if you let it soak more it will make the tea stronger).


 
Scylla
#7 Posted : 1/30/2020 9:53:04 PM
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The longer you leave the naptha in the pull the greater chance you will extract impurities like pigments. The red gunky stuff.

Id just keep it simple, cut out the water washes. Find a good a balance of water to base. Get it low. pH 13-14 or so. You can experiment. See what pH is best. Add the bark. Shake it up. Let it sit for at least 2 hours.

Add naptha. Shake it up. Let it phase out. Decant as soon as it does so. Repeat 3-4 times. Either combine your pulls or leave them separate, separate at first to see the yield and quality from each pull. Small volumes are best for high quality xtals. Place them in a freezer. The lower the temp setting on your freezer the better. Put it down as low as it can go. If it does 0 F do that. Check up on it 24 hours later and there should be nice white xtals floating in the naptha and piled at the bottom. Decant naptha through filter. Unfold filter paper and et filter dry. Pour dry/wet xtals out onto something flat and clean. Let them dry to full dryness. Done.
 
chinkof
#8 Posted : 2/4/2020 8:54:03 PM

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Scylla wrote:
The longer you leave the naptha in the pull the greater chance you will extract impurities like pigments. The red gunky stuff.

Id just keep it simple, cut out the water washes. Find a good a balance of water to base. Get it low. pH 13-14 or so. You can experiment. See what pH is best. Add the bark. Shake it up. Let it sit for at least 2 hours.

Add naptha. Shake it up. Let it phase out. Decant as soon as it does so. Repeat 3-4 times. Either combine your pulls or leave them separate, separate at first to see the yield and quality from each pull. Small volumes are best for high quality xtals. Place them in a freezer. The lower the temp setting on your freezer the better. Put it down as low as it can go. If it does 0 F do that. Check up on it 24 hours later and there should be nice white xtals floating in the naptha and piled at the bottom. Decant naptha through filter. Unfold filter paper and et filter dry. Pour dry/wet xtals out onto something flat and clean. Let them dry to full dryness. Done.


Thanks for the tip! Deffo gonna try it out!

Does the dmt in the non polar, base mixture, travel really fast to the polar naphtha? That even though when mixing/stirring it up does capture all the DMT? I want to make an automated stirrer, with a timer on it. Does slow stirring for like 5 hours equal 8 hard stirs in 48 hours for example?

Also would it be worth to add for every 100ml of base water 10 grams of normal salt to help the polarity?

 
downwardsfromzero
#9 Posted : 2/4/2020 9:54:04 PM

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Think about the process. Stirring is done, in this instance, to maximise the ratio of contact area between the liquid phases and the volume of those liquid phases. As Scylla says, one really good stir should in theory do the trick. The remaining time in question is how long it takes for the two phases to separate.

Salt increases the polarity of the aqueous phase, helping to push non-ionic things (like DMT freebase) into the non-polar solvent. Salt is less soluble in lye solutions, due to the common ion effect.
Ora, lege, lege, lege, relege et labora

“To be GOVERNED is to be watched, inspected, spied upon, directed, law-driven, numbered, regulated, enrolled, indoctrinated, preached at, controlled, checked, estimated, valued, censured, commanded, by creatures who have neither the right nor the wisdom nor the virtue to do so. To be GOVERNED is to be at every operation, at every transaction noted, registered, counted, taxed, stamped, measured, numbered, assessed, licensed, authorized, admonished, prevented, forbidden, reformed, corrected, punished. It is, under pretext of public utility, and in the name of the general interest, to be place under contribution, drilled, fleeced, exploited, monopolized, extorted from, squeezed, hoaxed, robbed; then, at the slightest resistance, the first word of complaint, to be repressed, fined, vilified, harassed, hunted down, abused, clubbed, disarmed, bound, choked, imprisoned, judged, condemned, shot, deported, sacrificed, sold, betrayed; and to crown all, mocked, ridiculed, derided, outraged, dishonored. That is government; that is its justice; that is its morality."
― Pierre-Joseph Proudhon
 
chinkof
#10 Posted : 2/5/2020 7:16:42 PM

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downwardsfromzero wrote:
Think about the process. Stirring is done, in this instance, to maximise the ratio of contact area between the liquid phases and the volume of those liquid phases. As Scylla says, one really good stir should in theory do the trick. The remaining time in question is how long it takes for the two phases to separate.

Salt increases the polarity of the aqueous phase, helping to push non-ionic things (like DMT freebase) into the non-polar solvent. Salt is less soluble in lye solutions, due to the common ion effect.



I get the idea that one good stir theoretically should do the job... But my thought was that dmt has some "travelling time" to travel from the polar to the non polar solvent. For example if two cars parked next to each other and you (the driver) needs to switch cars, the switch takes time. My thought was that the dmt needs a couple of sec to travel between the solvents. So even though theoretically it should be doable in one pull because of this travel time some dmt will still remain in the polar solution. Or is this time so small that it shouldn't be a thing to think about?


I know that you will not be able to dissolve the same amount of salt in a lye solution, but maybe even the smallest amounts of salt will help? What do you think? Any experience with this?
 
 
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