First extraction, a-nitrile-ated...

[dooby]

Hello,

My first ever extraction on 100 gr of powdered mhrb was reasonably successful with room-temperature precipitation on pulls 1 and 2...

I am afraid, however, that I made a mistake and I am not sure if this will affect the quality of my yield and, if so, how to resolve the situation.

Being very apprehensive about the base/naphtha mixture touching any plastic or aluminium I came up with the idea to wedge one of my disposable nitrile gloves between the bottle and the cap which seemed to work like a charm...

After every shake/roll, said nitrile glove was removed from its position, rinsed and put aside until the next shake/roll (during separation bottle was "capped" with a small glass disc),

At the end of the day, no visible damage to the nitrile itself but I did notice quite a bit of discoloration (used to be blue, now a blue-ish white)...

My pull jar is still in the fridge and will remain there until no more crystal formation is noticed...

How should I proceed?

The tek I used was more or less Cybs hybrid salt tek...

PLUR

 

[dooby]

Nobody?

 

[JesusBuiltMyHotRod]

Unless you have a very good knowledge of chemistry and know how the nitrile could/would be effected by the napatha/base mixture I would consider it contaminated with the nitrile and/or whatever the blue coloring is. Unless someone with an advanced knowledge of chemistry advises differently I would have to say either discard it (safe than sorry!) or save it until you are sure it is unsalvageable.

If you do decided to finish the extraction and use it, please do not share the risk or the spice with anyone. You may do as you wish with your own body but please don't take chances with others.

Good luck with whatever route you choose.

 

[dooby]

I will not use any of this spice, nor will I offer it to anyone else until I know it's safe or until I know how to clean it...

Every bottle I found so far has either a plastic cap or an aluminium one, so which should I use?

 

[Du57mi73]

Pickle jars are good. The large 84oz ones are what I use. 4$ and you get some pickles too!

Blue is bad. Don't use that. Id dump it. If you realllllllly insist on using it then I would do multiple clean up steps til it has absolutely no blue. Personally I wouldn't even risk it.

 

[cyb]

Every bottle I found so far has either a plastic cap or an aluminium one, so which should I use?

Use any bottle you like... Carve yourself a cork.

 

[JesusBuiltMyHotRod]

Try regular mason jars with a smoothed sheet of aluminum to act somewhat like a gasket preventing the lid from contacting the jar lid. Always has worked for my friend and has no evidence of contamination, but then again he doesn't use napatha/lye so take that info however you wish.

Next time try using whatever material in a "dry run" with no plant matter first to see if the selected material is reactive with whatever solvent/extraction route you choose. It's better to lose some time now than your entire yield later.

EDIT: Cork should work well also. If I'm correct it will be somewhat absorbant but relatively non reactive. If it does react it's breakdown products shouldn't be anymore harmful that what the root bark produces.

 

[Du57mi73]

I've thought about cork, didn't know how long it would survive ph14 though.

Do NOT use aluminum with hydroxides. It creates hydrogen gas and will explode your jar.

 

[JesusBuiltMyHotRod]

Do NOT use aluminum with hydroxides. It creates hydrogen gas and will explode your jar.

Always good to know. My bad.

 

[benzyme]

nitriles are colorless. what you're seeing is pigment, large molecules.
you can freeze precipitate the naphtha, then filter.
then I'd suggest dissolving the crystals in room temp ethyl acetate, and filtering through a thin layer of activated carbon, and keep rinsing with ethyl acetate.

 

[dooby]

Well, I noticed the discoloration of the nitrile glove, but my yield itself is colorless...

I will get some activated carbon and will try to find some ethyl acetate to perform the wash just to make sure my spice is void of any impurities...

Is it okay to use a coffee filter to hold the activated carbon or will it also trap wanted molecules?

Also, I finally found a way to mix my basic solution and solvent without any risk of contamination... I feel silly for not having thought of this much earlier... I am going to use two bottles, basic solution in one, solvent in the other, pour basic solution into/onto solvent using a stainless steel funnel, let separate... If you want to mix more than once simply funnel back into first bottle... Small glass discs are used to "cap" the bottles while the solvet is seperating, any pressure build up will "lift" the disc thus releasing pressure... By funneling the neck of the bottle stays clean (as opposed to when shaking etc) making pipetting off the solvent that much easier for those with bad Eyesight such as myself

PLUR

 

[dooby]

Hello,

After reading up on different re-x and washing procedures I have come up with some ideas on how to proceed, and some questions too...

About the ethyl acetate/activated carbon wash:
1: Will the freebase molecules turn into an acetate?
2: I read that ethyl acetate reacts with both water and NaOH so I suppose my only option after the filtration would be to evap the ethyl acetate, is this correct?
3: Assuming "yes" to both 1 and 2, how should I proceed after the evaporation? Basify with sodium bicarbonate, pull with hot naphtha, then let separate or filter?
4: "Keep rinsing"? Does this mean pouring additional ethyl acetate onto/through the activated carbon after the ethyl acetate/dmt solution has passed through the filter?

About filtering:
5: When a solution containing dmt is passed through a coffee filter, will the filter trap any dmt-molecules? Is there a difference between freebase, fumarate or acetate molecules of dmt in this regard?

Due to my bad eyesight I cannot be 100% sure that no basic solution was pulled so I would like to do some wash as well. Right now my yield is drying on the bottom of my precip jar so I am thinking of combining re-x and wash then doing the ethyl acetate/activated carbon filtration afterwards. I am thinking of dissolving everything in hot naphtha, allow impurities to settle (keeping naphtha hot), then decanting, then washing with sodium (bi?)carbonate. I think I'll use 1/5 of sodium (bi?)carb saturated solution compared to naphtha volume...
6: Why should the sodium solution be cold?

Thank you for reading this and sharing your knowledge, whoever you are

PLUR

 

[Randomness]

If you want to make a good gasket just buy an appropriately sized bit of PTFE sheet of e b a y and cut it into shape. That will beat any old gloves and is used in labs.

 

[benzyme]

Hello,

After reading up on different re-x and washing procedures I have come up with some ideas on how to proceed, and some questions too...

About the ethyl acetate/activated carbon wash:
1: Will the freebase molecules turn into an acetate?
2: I read that ethyl acetate reacts with both water and NaOH so I suppose my only option after the filtration would be to evap the ethyl acetate, is this correct?
3: Assuming "yes" to both 1 and 2, how should I proceed after the evaporation? Basify with sodium bicarbonate, pull with hot naphtha, then let separate or filter?
4: "Keep rinsing"? Does this mean pouring additional ethyl acetate onto/through the activated carbon after the ethyl acetate/dmt solution has passed through the filter?

About filtering:
5: When a solution containing dmt is passed through a coffee filter, will the filter trap any dmt-molecules? Is there a difference between freebase, fumarate or acetate molecules of dmt in this regard?

Due to my bad eyesight I cannot be 100% sure that no basic solution was pulled so I would like to do some wash as well. Right now my yield is drying on the bottom of my precip jar so I am thinking of combining re-x and wash then doing the ethyl acetate/activated carbon filtration afterwards. I am thinking of dissolving everything in hot naphtha, allow impurities to settle (keeping naphtha hot), then decanting, then washing with sodium (bi?)carbonate. I think I'll use 1/5 of sodium (bi?)carb saturated solution compared to naphtha volume...
6: Why should the sodium solution be cold?

Thank you for reading this and sharing your knowledge, whoever you are

PLUR

1. no. ethyl acetate isn't the same as acetic acid.
2. ethyl acetate may react with strong base or strong acid, but the reaction only occurs when the solution is heated.
3. you may salt the ethyl acetate, or evaporate...just like you would with naphtha.
4. yes.
5. not really, especially if DMT is in a free base form. if it is a free base, the molecule is uncharged, and will have little interaction with cellulose. salts on the other hand, are products of charged species, and in a polar solution, those species may be retained more readily on the cellulose; this is especially true of fumarate and acetate molecules, but for another reason...they have OH groups, which can interact with OH groups on cellulose.
6. it doesn't matter if the sodium carb/bicarb solution is cold, it can be room temp.

 

[dooby]

Thank you benzyme,

As for question 1, I was afraid that the ethyl acetate might affect the molecule due to it's pH of 5-7 (couldn't find a more specific number)...

I will proceed as planned and post the results when I have them... procuring ethyl acetate might take some time though...

PLUR

 

[JesusBuiltMyHotRod]

This is starting to sound WAY more expensive than starting again with new material but I'm definitely learning some.

 

[arcologist]

Why don't you take your naphtha, add FASA, collect and dry the precipitated DMT fumarate, then base and pull again with fresh naphtha? That should remove most if not all of the nitrile impurities and shouldn't take more than a few hours.

 

[dooby]

This is starting to sound WAY more expensive than starting again with new material but I'm definitely learning some.

Starting a new extraction would be easier, cheaper and less time-consuming but on the other hand this was my first ever yield so trying to save it is not only a matter of priciple but it's also fun and educational...

 

[Du57mi73]

Yea man, start over. Lol. Uphill battle all the way.

Ps, nice punwork on the title of the thread.

 

[dooby]

Why don't you take your naphtha, add FASA, collect and dry the precipitated DMT fumarate, then base and pull again with fresh naphtha? That should remove most if not all of the nitrile impurities and shouldn't take more than a few hours.

Where I live fumaric acid seems to be quite hard, if not impossible, to find OTC...

It's not even in the list of chemicals my pharmacist can order

I am not sure if it's safe to order fumaric acid online from an official chem supplier...

I am now researching the possibilty of back-salting with vinegar...

Also, the one place I found that sells ethyl acetate is a paint supply shop, but they are also selling some watched chemicals so I'm a bit apprehensive about shopping there and still looking for a safer option...

PLUR