Crystals at the bottom of sep funnel

[Sigtyr]

Greetings!

Long time lurker first time poster.

I thought I would share my dismal attempts at an A/B extraction and would appreciate any feedback regarding the below mentioned crystals that formed at the bottom of the separatory funnel. A lot went on during this whole process so I'll just gloss over it without going into too much detail.

A couple of months ago I harvested some twigs/undergrowth from Acacia Acuminata and long story short, followed a combination of instructions from the DMT Handbook and the Elf Spice tek, though choosing to use glassware over HDPE plastics and what not.

I used Phosphoric acid for the soak/cook with 100g of the acacia bark, NAOH for basifying, Xylene for the defat and Shellite for the pulls and did a water wash with sodium carbonate.

Basically I yielded nothing from my first attempt. The shellite took on a slightly yellow colour after each separation but did not turn cloudy after reducing via evaporation. Freeze precipation resulted in nothing also (3 days in the freezer.)

I know acacias are variable and the day I harvested this particular tree it was cold and wet and the tree was also in bloom so I figured this could have had an impact on alkaloid content.....or maybe I just screwed it up.

Anyway I tried again with some left over bark from the harvest. This time I left out the defatting with Xylene and the sodium carbonate wash and was a bit more aggressive with the mixing of the basified soup and shellite… in fact I shook the living shit out of it each time just out of frustration as I figured I had nothing to lose!

After letting it settle for a few days as there was quite a lot of froth etc, I noticed the shellite again had taken on that slightly yellow colour and this time a whitish oil layer was sitting between the shellite and water. I drained off the soup and then collected the oily white liquid and the shellite into a beaker and repeated this a couple more times.

Still not convinced that I was having much success I decided to add more NAOH to the soup, poured it into a sep funnel, added some shellite and shook the shit out of it again and left it over night.

The next day I checked and there was no white oil between the layers, this time however, lots of crystal shards had formed and were sitting at the bottom of the sep funnel which almost blocked it up and made draining the soup very slow though I managed to get it all out (aside form the crystals and shellite).

The next thing was to try and get the crystals out, so I made a hot water bath and let the funnel soak in that until the crystals dissolved then drained it into the beaker containing the previous pulls. I have now poured all those contents into a glass tray and will let it slowly evaporate and see what happens.

I am not convinced that those crystals are DMT, I'm leaning towards them being NAOH? Has anyone else experienced this?

Thanks for reading.

Here is a pic of aforementioned crystals in the sep funnel


Dissolved crystals, white oil and shellite



After this I think my next attempt will be on Acacia Floribunda ,maybe ill have more luck with that. I couldn't do any worse HA!

 

[Sigtyr]

Crystals at the bottom

 

[atomu235]

Depends on how much NaOH you actually added in. Excess that couldn't dissolve in water would precipitate out of solution. NaHO solubility in shellite (naphtha) would be minimal. It's also a bit odd that your aqueous solution did not turn darker after adding in NaOH. Mine always go very dark, black almost.

You can easily test if it's NaOH by pH test. You could also do a flame test. Sodium ions will give you a yellow-ish flame.

I'd also be inclined to think it's NaOH as there seems to be a lot of it. Much more than the possible alkaloids...? Besides alkaloids would dissolve in the non-polar solvent on top, not drift to the bottom.

My suggestion - start over again. Experiment and learn

 

[downwardsfromzero]

NaOH is ludicrously soluble in water, you might be seeing a sodium salt of some plant-based acid. A few simple physical tests would set you in the right direction. DMT freebase has a melting point in the range 46 - 60°C or thereabouts, depending on the polymorph. It also has a characteristic odour in the range of mothballs/plasticky/"new sneakers" to floral/fruity when exceptionally pure :want:

DMT crystals would dissolve in fresh naphtha (or whatever NPS you're using) - so, don't throw anything away yet!! You still have a chance of finding out whether there's anything of value in your plant extraction.

The golden rule is NEVER throw anything away until you're sure you've got the goods!!

 

[Sigtyr]

Depends on how much NaOH you actually added in. Excess that couldn't dissolve in water would precipitate out of solution. NaHO solubility in shellite (naphtha) would be minimal. It's also a bit odd that your aqueous solution did not turn darker after adding in NaOH. Mine always go very dark, black almost.

You can easily test if it's NaOH by pH test. You could also do a flame test. Sodium ions will give you a yellow-ish flame.

I'd also be inclined to think it's NaOH as there seems to be a lot of it. Much more than the possible alkaloids...? Besides alkaloids would dissolve in the non-polar solvent on top, not drift to the bottom.

My suggestion - start over again. Experiment and learn

The solution was black when it was first basified (see attached picture), but after I failed to pull anything from it I poured it all back into the sep funnel and re-added the used naptha and let it sit in the dark for several weeks....basically until I felt like having another crack at it rather throw it out just in case I missed something. Maybe that had something to do with the colour changing back to a red?

The contents of the tray has now solidified so I will post some pictures of that and I will also try some of those tests you suggested. Thanks for your input.

 

[Sigtyr]

NaOH is ludicrously soluble in water, you might be seeing a sodium salt of some plant-based acid. A few simple physical tests would set you in the right direction. DMT freebase has a melting point in the range 46 - 60°C or thereabouts, depending on the polymorph. It also has a characteristic odour in the range of mothballs/plasticky/"new sneakers" to floral/fruity when exceptionally pure :want:

DMT crystals would dissolve in fresh naphtha (or whatever NPS you're using) - so, don't throw anything away yet!! You still have a chance of finding out whether there's anything of value in your plant extraction.

The golden rule is NEVER throw anything away until you're sure you've got the goods!!

I have absolutely no idea what I have here, but there is definitely an odour to it that I would associate with "new sneakers". Maybe that's wishful thinking on my part but I really couldn't think of any other way to describe the odour...perhaps it's a residual odour from shellite/naptha?.

Anyway, I'm certain this is a failed experiment but I'll try the above mentioned tests, and worse case I'll put it down to a learning curve and try another Acacia species.

Thanks for your reply.

 

[Sigtyr]

This is what was left after the evaporation. It has an oily/waxy feel to it.

 

[atomu235]

downwardsfromzero might be onto something here. It could be some sodium salt... No easy way to find out the structure using diy though afaik.

Do a flame test, ph test and melting point test (can be done reliably and easily @ home using a Thiele tube). To purify you may want to re-crystallize from solvent.

Just by looking at the end product it looks like a crude full spectrum extract. Looks can be deceiving though, make sure you have no NaOH left in it. A water wash will get rid of water soluble salts and NaOH easily (DMT freebase solubility in water is minimal). After drying dissolve end product in a non-polar solvent, filter, re-x and test. Your yield may/will go down but it will def be more pure.

Ps. I describe the smell of pure DMT as my grandma's wardrobe (aka mothballs). I can't get rid of this connection from my mind ;-)

Pps. From pick I'm assuming you have access to basic labware. Try to use single component solvents [pentane, hexane, heptane or for ex toluene 'non selective']. You never really know what's inside shellite (aka naphtha). Colorimetric test thread might also come in handy: Colorimetric test results (Marquis, Mecke, Ehrlich, etc) for different alkaloids - Plant Analysis and Substance Testing - Welcome to the DMT-Nexus

 

[downwardsfromzero]

The stuff on the upper right of the picture looks 'OK', the more powdery looking stuff to the left is contaminated with some kind of plant salts. Recrystallise using a pure hydrocarbon - heptane is good - or perhaps dissolve in vinegar, etc. for a mini A/B clean up.

 

[atomu235]

The stuff on the upper right of the picture looks 'OK', the more powdery looking stuff to the left is contaminated with some kind of plant salts.

Well spotted.

 

[Sigtyr]

downwardsfromzero might be onto something here. It could be some sodium salt... No easy way to find out the structure using diy though afaik.

Do a flame test, ph test and melting point test (can be done reliably and easily @ home using a Thiele tube). To purify you may want to re-crystallize from solvent.

Just by looking at the end product it looks like a crude full spectrum extract. Looks can be deceiving though, make sure you have no NaOH left in it. A water wash will get rid of water soluble salts and NaOH easily (DMT freebase solubility in water is minimal). After drying dissolve end product in a non-polar solvent, filter, re-x and test. Your yield may/will go down but it will def be more pure.

Ps. I describe the smell of pure DMT as my grandma's wardrobe (aka mothballs). I can't get rid of this connection from my mind ;-)

Pps. From pick I'm assuming you have access to basic labware. Try to use single component solvents [pentane, hexane, heptane or for ex toluene 'non selective']. You never really know what's inside shellite (aka naphtha). Colorimetric test thread might also come in handy: Colorimetric test results (Marquis, Mecke, Ehrlich, etc) for different alkaloids - Plant Analysis and Substance Testing - Welcome to the DMT-Nexus

I'll give the water wash and re-x a go and see how it looks and then maybe the mini A/B as suggested by downwardsfromzero. Would you suggest water washing with sodium carbonate or just water on its own?

Yes I have access to basic labware but unfortunately obtaining solvents such as toluene and heptane is not as easy as it once was in this part of the world (Australia). Shellite, xylene and d-limonene can be acquired from most hardware stores but aside from that we don't seem to be spoilt for choice down here, though I am looking into possible sources/options.

 

[Sigtyr]

Ok, so once water was added to this substance it all dissolved into a cloudy mess (pic attached).

Using a digital meter, I tested the PH which was fluctuating between 10.5 - 11.5 and also tested with litmus strips which also showed in the high end of things (12-13).

I then added vinegar until I got a PH of around 3-4 and once I added a little bit of NAOH solution to it and instantly, it looked as if it were forming crystals/emulsion (pic attached) similar to what had been found at the bottom of the sep funnel so I'm not sure what's going on but I tend to agree with you guys in that it is probably just some plant salt that has been extracted.

I have also added some shellite to it and I will leave it overnight and see what tomorrow brings, but I really don't think there is anything worthwhile too find in this batch.

Today I harvested some Acacia Floribunda bark so I'll attempt an extraction on that in the coming days and hopefully that will be more rewarding.

 

[atomu235]

It was an interesting experiment at least

Look up beauty, minerals shops, sports and performance, food additives shops, aquatic life shops, home and garden, paint supplies.

Two stellar examples over here in the UK:

https://www.minerals-water.co.uk

APC Pure

Simplicity for Science

apcpure.com

There may be similar alternatives over in Australia for DIY as well...? You'll need to find that out.

Ps. Do go back to this species once you have good solvents. Toluene can do miracles for pulling full spectrum alkaloid, hexane and heptane for purification of DMT (or direct extraction with basified water extract).

 

[Sigtyr]

It was an interesting experiment at least

Look up beauty, minerals shops, sports and performance, food additives shops, aquatic life shops, home and garden, paint supplies.

Two stellar examples over here in the UK:

https://www.minerals-water.co.uk

APC Pure

Simplicity for Science

apcpure.com

There may be similar alternatives over in Australia for DIY as well...? You'll need to find that out.

Ps. Do go back to this species once you have good solvents. Toluene can do miracles for pulling full spectrum alkaloid, hexane and heptane for purification of DMT (or direct extraction with basified water extract).

Thanks for the tips, I'll check out what's around. As a side note, I was just browsing those links you provided and I noticed that some of the products on there would be restricted from sale here (and watched) or at the least you would need to fill out an EUD.

It just goes to show how much of a "nanny state" Australia has become in recent years, hell as of Feb 2018, you cant even buy anything that contains codeine (headache tablets for example) without a prescription anymore. It's ridiculous.

Anyway back on topic; I plan on having another attempt at extracting from that particular Acacia Acuminata tree but I will wait until Jan-Feb when its much hotter, and hopefully that will improve the alkaloid content.

Thanks again for your input and advice, its appreciated.

 

[padawan]

Anyway back on topic; I plan on having another attempt at extracting from that particular Acacia Acuminata tree but I will wait until Jan-Feb when its much hotter, and hopefully that will improve the alkaloid content.

Thanks again for your input and advice, its appreciated.

Yeah, the land down under is not the best for this kind of science. However, some people will say that Acacia Acuminata, Vinegar, Shellite, Kalkwasser all work fairly well together using a standard dry-tek like Q21Q21's fluffy white, although AA is highly variable (0.3 - 1.3% or thereabouts from collected bark). Some might suggest lengthy acid soaks and long/hot pulls are also necessary. Same people might have had mixed experienced with NaOH and wet-teks, such as strange precipitates. Good luck, mate. :thumb_up:

 

[Sigtyr]

Anyway back on topic; I plan on having another attempt at extracting from that particular Acacia Acuminata tree but I will wait until Jan-Feb when its much hotter, and hopefully that will improve the alkaloid content.

Thanks again for your input and advice, its appreciated.

Yeah, the land down under is not the best for this kind of science. However, some people will say that Acacia Acuminata, Vinegar, Shellite, Kalkwasser all work fairly well together using a standard dry-tek like Q21Q21's fluffy white, although AA is highly variable (0.3 - 1.3% or thereabouts from collected bark). Some might suggest lengthy acid soaks and long/hot pulls are also necessary. Same people might have had mixed experienced with NaOH and wet-teks, such as strange precipitates. Good luck, mate. :thumb_up:

Interesting. I think I'll look into that tek and try it with Acacia Floribunda :thumb_up: