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benzyme
#141 Posted : 6/14/2015 8:32:17 PM

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my storage tank holds 20 lbs, i'll use a transfer tank that will hold about 5. my collection vessel is 3" O.D. x 12" , 0.065" wall thickness, with a 140 psi blow-off valve. all swagelok 1/4" fittings rated for 3000 psi , and needle valves rated for 6000 psi.
i'll only be operating at around 1500. I'll use a bath scale to weigh the cylinders.

co2 is relatively cheap, so i don't particularly care if i have to make trips to the welding supply shop.

the tricky part is going to be my implementation to the system, using an LC pump to inject ethanol. this isn't mentioned in any of the SFE blogs. i'm using a 1/16" O.D. to 1/4" NPT adapter, connected to a 1 psi check valve in 1/4" NPT cross.

I come from a background, academically and professionally, of method development (this is pure science). I'll also implement this in my hobbies.


"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 

Explore our global analysis service for precise testing of your extracts and other substances.
 
Nathanial.Dread
#142 Posted : 6/14/2015 9:33:58 PM

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Maybe one day when I'm living in one place for longer than about six months at a stretch.

Blessings
~ND
"There are many paths up the same mountain."

 
benzyme
#143 Posted : 6/14/2015 10:18:06 PM

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Thumbs up

I hear that
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
BongWizard
#144 Posted : 6/14/2015 11:05:46 PM

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benzyme wrote:
my storage tank holds 20 lbs, i'll use a transfer tank that will hold about 5. my collection vessel is 3" O.D. x 12" , 0.065" wall thickness, with a 140 psi blow-off valve. all swagelok 1/4" fittings rated for 3000 psi , and needle valves rated for 6000 psi.
i'll only be operating at around 1500. I'll use a bath scale to weigh the cylinders.

co2 is relatively cheap, so i don't particularly care if i have to make trips to the welding supply shop.

the tricky part is going to be my implementation to the system, using an LC pump to inject ethanol. this isn't mentioned in any of the SFE blogs. i'm using a 1/16" O.D. to 1/4" NPT adapter, connected to a 1 psi check valve in 1/4" NPT cross.

I come from a background, academically and professionally, of method development (this is pure science). I'll also implement this in my hobbies.


In my mind, using a transfer tank further reduces efficiency. Your supply pressure is limited to around 2800-3000psi, by adding an extra 5 lb tank into the line you're giving the gas more room to expand thus wasting more CO2 as overhead. Quick calculation leaves about 8.5 lb in the combined tanks at critical pressure, at which point that gas is useless for SFE. I know I'm probably being overly picky, but I'm looking at this from an engineering standpoint (which means efficiency is king).

Ethanol injection will be tricky. As I imagine your setup, if using a check valve rather than a machined mixer, the ethanol will have to be injected at a higher pressure the the CO2. This is well within the realm of many hplc pumps, but you haven't specified the pump so I just figured I'd mention that (though you probably thought of that already). A control valve on the CO2 inlet side of that union may also be useful for ensuring thorough mixture by partially disrupting the flow of CO2. It's probably best to mount the mixture union such that the ethanol inlet is slightly higher than the CO2 line (if not completely vertical, depends on the style of check valve).

Also, I see you haven't mentioned an extraction vessel as yet. Do you have one in mind? Or still searching? I can think of a fairly easy way to modify a small gas cylinder, although particular care must be taken with respect to the locking mechanism and associated seals. Otherwise one could manufacture one from appropriately sized stainless steel pipe (probably couldn't work a quick release into this, but the threaded seals could be more reliable, if a little tedious).
"Laws alone can not secure freedom of expression; in order that every man present his views without penalty there must be a spirit of tolerance in the entire population." -Albert Einstein


I'm not a big fan of SWIM. I mean, I've never met the guy, but any time I hear about him, he's doing something sketchy.
 
benzyme
#145 Posted : 6/14/2015 11:21:31 PM

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perhaps you are being overly picky, unnecessary. overthinking it.
the transfer is done thermodynamically, to the separate tank, no pump, with the plant material. the final transfer is also done thermodynamically (heating pad with therm controller, monitored with either the 3000 or 5000 psi gauges), to a lower pressure/temp vessel (I did mention, a sanitary 304 stainless spool, 3" x 12", with tri-clamps and 1/4" NPT ports/fittings, viton gaskets), with a pressure release valve. the ethanol injection is done before the initial CO2 transfer.
the other thing you're not taking into consideration is the immense utility of subcritical CO2 extraction. it has properties altogether different than supercritical, as it is the fluid phase of carbon dioxide.

do all the calculations if you want, but it won't tell you anything without an actual experiment; otherwise it's just mental masturbation. I've certainly given this some thought, with a couple years of consideration and reading electronic textbooks. just recently started purchasing everything.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
BongWizard
#146 Posted : 6/15/2015 1:46:30 AM

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I am familiar with the principles governing supercritical fluid extraction, but you were unclear about the arrangement of your particular setup. To me it sounded like you were proposing the use of the 5lb cylinder for gas transfer, but I now understand you intend to use it as your extraction vessel with the fitted stainless pipe acting as a fraction separator. And if the ethanol is injected before the introduction of CO2 (ie at 0 psig) then it shouldn't be overly complicated at all.



My understanding was that you were attempting to build a homebrew version of something more akin to the above diagram (less the CO2 pump and cooling system, obviously). I think I now understand what you're putting together, which leads me to think you may be overthinking it. If I'm understanding your setup correctly, I could assemble something equally functional (albeit, slightly less elegant) with about $50 worth of brass fittings, a length of stainless pipe, and a few bits of old welding kit (gauges, reg, hoses and a small oxy tank), give me 2 hours in the workshop and a cylinder of CO2 and it should be ready to go. No calcs this time, cuz this is just a bit of bush engineering Big grin
"Laws alone can not secure freedom of expression; in order that every man present his views without penalty there must be a spirit of tolerance in the entire population." -Albert Einstein


I'm not a big fan of SWIM. I mean, I've never met the guy, but any time I hear about him, he's doing something sketchy.
 
benzyme
#147 Posted : 6/15/2015 2:13:19 AM

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ok, now we're on the same page.
the heating pad with a PID controller is the thermodynamic variable, the needle valves are the control variables, and a stainless PTFE-lined hose handles the transfer. swagelok full-flow quickconnects attach to both tanks.

this is the simple transfer setup i'm looking at now, but will have a handtight nut for the transfer tank (the smaller one) shortly.

what isn't shown is the cross assembly to introduce the entrainer solvent. i'll integrate this in after I figure out the handtight nut into the app, as this will allow for convenient transfer of the plant material into the smaller tank.
the pump being used will be a Harvard Apparatus syringe pump with a glass BD syringe, not a high pressure HPLC pump.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
BongWizard
#148 Posted : 6/15/2015 2:35:13 AM

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Alright, now we're getting somewhere. Maybe we take this back to the advanced chem forum and unhijack the basic chem thread Laughing
"Laws alone can not secure freedom of expression; in order that every man present his views without penalty there must be a spirit of tolerance in the entire population." -Albert Einstein


I'm not a big fan of SWIM. I mean, I've never met the guy, but any time I hear about him, he's doing something sketchy.
 
JustCurious.
#149 Posted : 6/19/2015 2:46:55 PM

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Anybody interested in making a basic chemistry guide with me Smile

Would like to make a nice pdf with some pictures and reaction schemes if anyone is interested in contributing Smile
 
BongWizard
#150 Posted : 7/6/2015 7:29:18 PM

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JustCurious. wrote:
Anybody interested in making a basic chemistry guide with me Smile

Would like to make a nice pdf with some pictures and reaction schemes if anyone is interested in contributing Smile


What did you have in mind? What I mean is, the basics are fairly well covered, what do you think needs to be added/improved upon?
"Laws alone can not secure freedom of expression; in order that every man present his views without penalty there must be a spirit of tolerance in the entire population." -Albert Einstein


I'm not a big fan of SWIM. I mean, I've never met the guy, but any time I hear about him, he's doing something sketchy.
 
JefFlux
#151 Posted : 5/24/2017 2:10:01 AM

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Simple enquiry here. various teks for Acacia list Ph at 3-5 or 4 for the acidification stage. My question is will going below this to say ph 3 affect the formation of dmt salts in this phase ?
thanks in advance
 
Mindlusion
#152 Posted : 5/24/2017 4:35:39 PM

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JefFlux wrote:
Simple enquiry here. various teks for Acacia list Ph at 3-5 or 4 for the acidification stage. My question is will going below this to say ph 3 affect the formation of dmt salts in this phase ?
thanks in advance


it will not
Expect nothing, Receive everything.
"Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). "
He alone sees truly who sees the Absolute the same in every creature...seeing the same Absolute everywhere, he does not harm himself or others. - The Bhagavad Gita
"The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
 
chr0nic
#153 Posted : 5/1/2020 11:03:35 AM

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Hey Smile

I am about to try my hand at an ACRB extraction.

I'm buying a bunch of nice glassware second hand- it also comes with a Kartell Labware Autoclavable Pipette. I didn't have a glass pipette- it is something I need- and I wondered if it might work? I've read plastic isn't recommended for teks involving solvents, but I wondered if a chemists pipette would stand up to this?

"the robust structure of the body ensures high mechanical and chemical resistances, making them totally autoclavable at +121°C for 20 minutes"

Of course, I don't expect anyone here to be an expert in this... but if you are Thumbs up



If I can't use it then I'll just have to source another one... the rest of the glassware is still going to be awesome.
-Trillium-
 
chr0nic
#154 Posted : 5/1/2020 11:11:23 AM

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Here's the glassware... I'm thinking I may be able to use the 'burettes' if I can find that rubber oval type thing from somewhere Confused

-Trillium-
 
Brennendes Wasser
#155 Posted : 5/1/2020 7:01:16 PM

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That rubber thing you seek is called Pileus Ball, should not be too expensive to get! And you initial question was if these pipettes could be indeed used for an ACRB extraction?

And you say you will need a glass pipette - but at what step or for what actually? They are of course used where very precise dosage of liquids is crucial - I could only imagine this could be the case when applying concentrated hydrochloric acid to acidify the mixture - in any other cases you deliver very big volumes of any liquid, so I cant imagine what to do with them.

But in any case:

These pipettes are always used with disposable 1-way-use plastic attachments as their notch to pump up and deliver the liquids. And these are indeed not resistant against strong organic solvents like DMF or maybe THF? Not too sure, but at least they are totally resistant against any liquid that you would use in a regular TEK: (strongly) acidic water and hydrocarbons (Naphtha, Hexane, Heptane, ...). Therefore there is no restriction when doing regular root bark business and you could use both just right away.
The glass ware is of course not that accurate, but I think you would not even need any of these 2 for a regular TEK? Still I would go with the glassware, as it is a much sumpler mechanism and therefore more resistant to damage - unless you drop it - and also does not need constant supply of additional goods (that plastic tips of the mechanic pipettes) Thumbs up
 
Tony6Strings
#156 Posted : 5/1/2020 7:11:56 PM

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If you want a pipette for pulling solvent from a rootbark extraction, I advise getting a volumetric pipette. They come in various sizes, grab a 25 or 50 ml, also the red rubber bulb for the end. Mine was around $20 with a couple bucks for the bulb, from Carolina Biological.
olympus mon wrote:
You need to hit it with intention to get where you want to be!

"Good and evil lay side by side as electric love penetrates the sky..." -Hendrix

"We have arrived at truth, and now we find truth is a mystery- a play of joy, creation, and energy. This is source. This is the mystic touchstone that heals and renews. This is the beginning again. This is entheogenic." -Nicholas Sand
 
StarButterfly
#157 Posted : 5/10/2020 10:03:00 AM

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I have an harmala extract by manske. I need to clean it of protein residues due to allergies.
I want to dissolve it in water and cook for 4 hours.
Is it worth adding citric acid, lemon juice or vinegar? How much vinegar can you drink safely?
The protein structure is quite stable, as the extract received 8 hours.
 
Jees
#158 Posted : 10/19/2020 10:09:48 PM

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Love this channel, as he builds up his story he runs into practical aspects that are not part of the dry theory.
 
monomind
#159 Posted : 4/25/2021 1:38:09 PM

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A question if I may... Smile
Both h2o and acetone are polar solvents, so why is freebase dmt soluble in one but not the other ?

Thanks
 
benzyme
#160 Posted : 4/25/2021 3:03:38 PM

analytical chemist

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monomind wrote:
A question if I may... Smile
Both h2o and acetone are polar solvents, so why is freebase dmt soluble in one but not the other ?

Thanks



because whereas water is completely polar (has a stronger dipole) and can only participate in hydrogen-bonding, acetone has an isopropyl backbone, which allows it to engage in VDW interactions, as well as hydrogen-bonding (with the oxygen).
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
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