A/B EXTR. ADVICE?

[Spock's Brain]

Folks, a friend is considering doing another A/B extraction on some MHRB and would like some advice on some info he read in an extraction TEK that He recently read. This time He's going bigger, and for as close to transluscent crystals as possible, as opposed to an oily residue of insufficient quantity to re-crystalize.

1. An acid phase PH of 6 is purported to be sufficient to dissolve DMT, but leave other substance un-dissolved. Is a PH of 6 sufficient, or optimal? He had previously extracted at a PH of 2.

"pH of 6 is used because this is the highest pH that will ionise the DMT, and because it is not so low as conventional techniques use, it will not dissolve anything with a pKa lower than DMT."

2. He's planning on using ACETIC acid, instead of HYDROCHLORIC. Learning that Acetic being volatile, as opposed to more stable Hydrochloric, He's planning on reducing the acid phase to a more managable size, using a double boiler method, as the acetic is purported to "boil off," and not concentrate lowering the PH even more. Also, possibly needing less basification efforts. What's the best available form of ACETIC to use? Also, He wants to remove the concentrated acid from His domain. Overall, more managable volume, advice?

3. "aromatic" (turpentine, xylene) solvents are suggested to be used to wash, ie. defat the acid phase. the "aromatic" solvents are purported to be more powerful to remove unwanted substances, followed by a naptha defat wash to also remove any residue of the prior solvents. Experiences?

"Aromatic solvents are suggested in this step because they dissolve more than any other nonpolar solvent, and thus clean the product more than ether, chlorinated solvents or naptha/shellite. Do a final wash using the solvent that will be used for extraction to remove any excess aromatics suspended in the solution. This is done to eliminate the majority of the high boiling aromatic solvent from the solution so when it is extracted the high boiling component of the solvent is reduced. If there is materials that boil at a significantly higher temperature than that of the DMT (ie much more than 65°C) the dmt will not crystallise or dry properly, as it will boil before the solvent it is mixed with. This is known as 'oiling out' and is best avoided if possible."

The advice my friend read is from Soma's Complete Acacia TEK, maybe using MHRB so much defatting is not needed. He previously defatted with naptha His MHRB acid, and removed oily residue each time.

Advice, experiences? I'll post his results when he completes it. Also, he will attempt re-crystalization for first time, this time also.

 

[acolon_5]

1) a pH of 6 might be a bit on the high side. It will take longer to extract the goodies. If you are using naphtha (or equiv) you should end up with almost pure DMT. I would shoot for a little lower. At least 4

2) Glacial acetic acid is better than vinegar, but a little harder and more expensive to get. Vinegar works well and is what is most commonly used.

3) MHRB is a pretty low oil plant. Extensive defats are not really necessary. 1-2 defats will give clear spice. I have used Xylene (is stinks and is my least favorite), Toulene (strong, less smelly and is my favorite for defat) and naphtha (works well).

Good luck, I'm sure others have a lot of good tips to give. Read over the extraction help thread, you can see a variety of different opinions.

 

[69ron]

I love the "Spock's Brain" user name!!!! That's a really cool name.

Folks, a friend is considering doing another A/B extraction on some MHRB and would like some advice on some info he read in an extraction TEK that He recently read. This time He's going bigger, and for as close to transluscent crystals as possible, as opposed to an oily residue of insufficient quantity to re-crystalize.

1. An acid phase PH of 6 is purported to be sufficient to dissolve DMT, but leave other substance un-dissolved. Is a PH of 6 sufficient, or optimal? He had previously extracted at a PH of 2.

Bringing the pH down will extract more of some alkaloids and less of others. It all depends on the alkaloid in question.

Almost everyone is going to tell you to use pH 3-4. Extracting at pH 3-4 is the norm because some alkaloids have a low pKa and require that range. Also, some alkaloids are more soluble in dilute acids, but some are less so. For example harmine HCl is more soluble in pure ware than in dilute HCl. If using a Soxhlet, that concept is almost completely irrelevant.

You should know that when shamans make water extractions of DMT plants, they don’t add any acids to adjust the pH. They simply boil the plant material in pure water and that is very effective.

DMT has a pKa of 8.68, meaning that at pH 6.68 99% is in water soluble salt form, and at pH 8.68 50% is, and at pH 10.68 99% is in freebase form. So at pH 6 more than 99% is in water soluble salt form so that’s the perfect pH to extract at using water, if the salt form is highly water soluble, but some are not. Diplopterys and Psychotria contain highly water soluble forms of DMT and so no pH adjustment is ever needed to extract the DMT.

With most plants you can extract nearly 90% of the DMT at pH 6 by simply boiling it 3 times in water for 30 minutes each time. SWIM extracts in a Soxhlet using 91% IPA for 12 hours without adding any acids and gets about 99% of all the DMT out of the plant material (this applies to Mimosa, Diplopterys and Psychotria). The leafy plant material usually has a pH of 5-6 naturally because of the acids present in the plant. This of course depends on the plant material in question. A lower pH is not needed unless the water solubility of the alkaloid salt present in the plant is very poor, and that all depends on what salt of DMT is present in the plant. Different salts have different solubility profiles. For example, DMT HCl is far more water soluble than DMT picrate.

"pH of 6 is used because this is the highest pH that will ionise the DMT, and because it is not so low as conventional techniques use, it will not dissolve anything with a pKa lower than DMT."

Yes. That is absolutely correct.

2. He's planning on using ACETIC acid, instead of HYDROCHLORIC. Learning that Acetic being volatile, as opposed to more stable Hydrochloric, He's planning on reducing the acid phase to a more managable size, using a double boiler method, as the acetic is purported to "boil off," and not concentrate lowering the PH even more. Also, possibly needing less basification efforts. What's the best available form of ACETIC to use? Also, He wants to remove the concentrated acid from His domain. Overall, more managable volume, advice?

HCl (hydrochloric acid) also boils away just like acetic acid, so there’s no advantage there. But HCl is more dangerous to use so it’s better to use acetic acid.

3. "aromatic" (turpentine, xylene) solvents are suggested to be used to wash, ie. defat the acid phase. the "aromatic" solvents are purported to be more powerful to remove unwanted substances, followed by a naptha defat wash to also remove any residue of the prior solvents. Experiences?

"Aromatic solvents are suggested in this step because they dissolve more than any other nonpolar solvent, and thus clean the product more than ether, chlorinated solvents or naptha/shellite. Do a final wash using the solvent that will be used for extraction to remove any excess aromatics suspended in the solution. This is done to eliminate the majority of the high boiling aromatic solvent from the solution so when it is extracted the high boiling component of the solvent is reduced. If there is materials that boil at a significantly higher temperature than that of the DMT (ie much more than 65°C) the dmt will not crystallise or dry properly, as it will boil before the solvent it is mixed with. This is known as 'oiling out' and is best avoided if possible."

SWIM says no. The best to defat with is DCM. DCM pulls out far more junk than solvents like xylene and it evaporates really fast, leaving no hidden residue like xylene. SWIM tested this and after all the xylene defats pulled out no more fats, DCM could still pull out a ton of more fats and oils. And of course if you plan to extract with naphtha, do a final defat with that solvent. But SWIM gets better results extracting with DCM and then doing a freeze precipitation with heptane. SWIM find naphtha to be a very poor extraction solvent.

The advice my friend read is from Soma's Complete Acacia TEK, maybe using MHRB so much defatting is not needed. He previously defatted with naptha His MHRB acid, and removed oily residue each time.

Advice, experiences? I'll post his results when he completes it. Also, he will attempt re-crystalization for first time, this time also.

Don’t skip the defat step if you want really clean results. MHRB has oils and fats in it. Its not as much as the leafy material, but it is there. However, most of the oils and fats in MHRB aren’t very soluble in heptane or naphtha. If the final dried extract is dissolved in a small amount of heptane or naphtha, most of the oils and fats won’t dissolve. The heptane/naphtha can then be poured off leaving behind the junk. Then the DMT can be freeze precipitated for a really clean end product. When freeze precipitating DMT, the defat step is not that important.

 

[extrememetal43]

http://forums.lycaeum.org/index.php/topic,23941.0.html

just wondering what u thot of these peoples opinion on using DCM.

 

[endlessness]

why doing a defat with mimosa?

I have thought about doing this, but it seems to me very unnecessary (feel free to disagree )

For doing a defat, one needs to use a considerable amount of solvent, and the results are not that substantial. Just look at all these white crystals people get without ever getting near the defat step

Instead of doing a defat, isnt it just soooooooo much better to make recrystallization? It cleans much more the spice and uses very very little solvent... plus its a fun process which you can play with and make your crystals grow larger if you want

 

[burnt]

why doing a defat with mimosa?

I have thought about doing this, but it seems to me very unnecessary (feel free to disagree )

For doing a defat, one needs to use a considerable amount of solvent, and the results are not that substantial. Just look at all these white crystals people get without ever getting near the defat step

Instead of doing a defat, isnt it just soooooooo much better to make recrystallization? It cleans much more the spice and uses very very little solvent... plus its a fun process which you can play with and make your crystals grow larger if you want

all depends when you want to clean up before or after with mimosa.

 

[69ron]

http://forums.lycaeum.org/index.php/topic,23941.0.html

just wondering what u thot of these peoples opinion on using DCM.

SWIM is very skeptical of that report. Here’s why.

* Hundreds of other professional extractions based on DCM fail to show the presences of N-chloromethyl-DMT. WHY IS THAT?

* N-chloromethyl-DMT is only generated in trace amounts according to the reports SWIM read, if they are true. SWIM tried specifically to make N-chloromethyl-DMT and can't seem to do it. Why can’t SWIM make it if it’s so easy to make?

* N-chloromethyl-DMT should be insoluble in naphtha/heptane and so it wouldn't make it into the final product when freeze precipitating in naphtha/heptane anyway. So who actually cares about that?

* When using DCM, SWIM always gets better yields than if he uses naphtha/heptane as the non-polar solvent, so he’s not about to switch to an inferior solvent just because of that report. Because SWIM freeze precipitates in heptane, it's not possible for N-chloromethyl-DMT to be present in his final product. And if any was generated at all, it is so small that it doesn't affect SWIM's yields at all.

SWIM has extracted DMT from Psychotria viridis using DCM and had it professionally analyzed after he read about that report. The results were that SWIM’s purified DMT crystals contained 98.7% DMT and 1.2% DMT N-Oxide. So that’s 99.9%. If there’s just 0.1% N-chloromethyl-DMT in it, which wasn’t detected, then who cares? SWIM surely doesn’t care.

If the sky is falling, and it really is falling, then there should be more evidence of it, not just two isolated reports. They could have done any number of things to cause N-chloromethyl-DMT to form. SWIM can’t make it and he tried. So there’s something missing in those reports. Their solvents may be contaminated or something else is amiss. Until SWIM can make it, he believes they did something special to cause it to form which they failed to add to their report. Otherwise why can’t SWIM make it too?

Also, why is it that in the report itself they are having difficulty detecting it? They seem unsure as to it’s existence and they don’t know exactly how it formed, they are just making guesses.

Where’s the solid evidence? Why can’t anyone else detect N-chloromethyl-DMT?

Man I love their statement, "Our recent research has confirmed that DMT reacts with dichloromethane (DCM), either as a result of work-up or storage to give a quaternary N-chloromethyl ammonium salt". They clearly state that they don't know if it even formed by their procedure or from storage conditions and yet they use the word “confirmed”! They give no actual proof. I want to see an exact procedure to produce it from pure DMT (not a plant extraction) and DCM that is reproducible by SWIM and others.

SWIM doesn’t take it seriously. Until someone can show SWIM a reliable method of making it that actually works, SWIM will consider it to be just another mistake in the history of mistakes reported by a few chemists out there monkeying around.

The report is full of too many holes. Someone needs to show exactly how to reliably create N-chloromethyl-DMT in a lab using pure DMT and DCM. The procedure SWIM saw doesn’t work.

In all likelihood the chemical was extracted from the plant, not generated in the extraction process and that’s why no one else can detect it. Sometimes chemicals are detected only in one batch of plant material, even when the same exact procedures are followed. For example, SWIM found large amounts of 5-MeO-DMT in Diplopterys cabrerana in one batch, and another batch contained absolutely no 5-MeO-DMT at all.

Maybe the plant was watered with chlorinated water and that caused the plant to make N-chloromethyl-DMT?

What I find amazing is that people will take a few isolated reports and start spreading them around the internet as if they have been proven to be facts. That’s a little scary.

EDIT: Has anyone else been able to successfully make N-chloromethyl-DMT from pure DMT and DCM? If so, exactly HOW? Step by step. What is the pH needed, what acid is needed, how much DCM, how much DMT, how long does the reaction take, what is the proper temperature, and what is the yield of N-chloromethyl-DMT? Are we talking something like a yield of 0.0004% or more like 99%?

 

[burnt]

SWIM would like to read that article and see what they did exactly. SWIM would agree the conditions necessary to do this in significant quantities would most likely not be those used by the average swim person.

SWIM would also like to add SWIM used DCM once and also tested purity on the batch and only spice showed up and a little oxide. well SWIM actually used a mix of solvents to see what separated the easiest but DCM was one of them.

 

[69ron]

Talking with another SWIM off-line, SWIM believes this unusual finding of chloromethyl-DMT is actually not caused by DCM but instead caused by DMT reacting with DCM that is contaminated with methyl chloride (chloromethane). Poorly made DCM often is contaminated with methyl chloride. If these researchers used cheap DCM, then this is probably the cause of their unique finding.

After all, this compound is chloromethyl-DMT, not dichloromethyl-DMT. If it were reacting with dichloromethane (DCM) I believe it should form dichloromethyl-DMT and not chloromethyl-DMT. This explains why no one else seems to be able to make chloromethyl-DMT by reacting it with DCM. Everyone else is using good quality DCM that is free of methyl chloride.

Page 29 of ECONOMICS BACKGROUND DOCUMENT found at http://www.epa.gov/epaoswer/hazwaste/id/chlorali/ca_ebd.pdf

commercial dichloromethane (methylene chloride) may contain up to 1.0% methyl chloride, chloroform, 1,1- dichloroethane, and 1,2-dichloroethene as impurities (WHO, 1986, p.45).

It must be the 1.0% methyl chloride in some DCM causing this reaction, not the DCM. Otherwise everyone would find chloromethyl-DMT in their DCM extractions and they clearly don’t. SWIM never found it. SWIM always buys 99.99% pure DCM. He doesn’t use lab grade. They probably used lab grade contaminated with methylene chloride.

After thinking about it and talking with others, SWIM is sure this is absolutely the cause. So SWIM recommends that you don’t use cheap lab grade DCM. Use good quality 99.99% DCM, not the lab grade stuff.

 

[burnt]

Interesting find! highlights importance of choosing your solvents wisely!