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Harm reducing chemistry question

Gnomelad

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Sep 24, 2016
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How would one extract a freebase alkaloid from diethyl ether or kerosene? Not sure if an evaporation would work if it's suspended in the solvent... Maybe to much would be lost... Trying to remove as much solvent or gas as possible... It's actually two questions... If another solvent is needed prefferably one that would seperate the alkaloid from the solvent or gas without being left in the end product...
 
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Add small portion of dilute hydrochloric in aqueous solution, or in methanol or other alcohol solution if the salt is soluble in such, this pulls it out into the aq. phase, extract 3x with portions of acidified polar solvent (a mix of alcohol and H2O can be good, that way evaps off faster) and combine the extractions after each time, in a closed sep funnel, turning end over end (DO hold the stopper in and make sure the valve tap is CLOSED. Easy to accidentally forget and have a nasty accident :p)

Combine the acidic extractions, keep the nonpolar phase until your done. Evap polar phase containing the salt. Or back-extract into a small volume of ether after basing again and evap. Kerosene is a nuisance, high boiling mixed aromatic-aliphatic alkanes. Use about 10% HCl for the salting unless of course another acid is chosen, either way about ten percent maybe 15.

Also the product can be somewhat acidey so you can also check PH once evaporated, or wash the salt with a little wee bit of very dilute bicarbonate solution, just a ml or two, dropwise on top until neutral, so it doesn't sting like a bastard when used. Keep your solvents until your done, and with valuble solvents, recycle. Making sure to test ether for peroxides with potassium iodide solution soaked into starched paper, if peroxides are present, they will oxidize iodide to I2 creating the violaceous-black color of iodine reacting with the starch. If present, then treat with either manganous (Mn++) or ferrous (not ferric) iron salts to decompose the peroxide, removing the ether from the resulting aldehyde product to prevent reformation of the peroxide. This should be doable with aq.bisulfite or metabisulfite salts to form the bisulfite adduct of the aldehyde and filtration.

Triphenylphosphine also works to deal with the peroxide rather than manganous manganese salts or ferrous iron. After treating, redistill, and test again with the iodide/starch papers. Personally I redistill the ethers under a pad of argon with a slow flow of argon gas to help discourage further peroxidation, also I sparge the ether, THF etc. using one of those fish tank airstones connected to the tubing to help force the residual O2 out of the ether solvent.

Don't distil ethers to dryness or let the pot go dry. Also don't distill to a tiny wee residual amount, leave a bit behind, because fully distilling to dryness concentrates the peroxides and intermediate hydroperoxides (although the hydroperoxides are much less nasty than the ethylidene peroxide or peroxides of other ethers.

Be ESPECIALLY careful with diisopropyl ether, its a notorious and nasty as hell peroxidizer, loves nothing better. Needs checking every three months rather than once a year for (new) ether. Its one to be careful with as it peroxidizes damned fast. THF needs checking once every 5-6 months or so in storage, more if your recovering and recycling.

The ether tailings, toss 'em out, soak onto paper and burn the buggers etc. AWAY from things that could be damaged.
 
Just evaporate the solvent on e.g. a water bath - whatever alkaloid you are working with should not be anywhere near as volatile as ether/naptha/kerosene. If you can't get the kerosene off you may need to do the acid-base extraction Limpet wrote.

somehow I don't think OP has access to triphenylphosphine either, if he's using kerosene :) - i prefer BHT or analogs anyway to stabilise ether - on a small scale just keep the ether wet and peroxide formetion will be retarded. Usually peroxide formation is not a problem with modern stabilised solvents btw.
 
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I took 'kerosene' to mean high-boiling naphtha in the form of mostly aliphatics but with a nevertheless significant level of aromatics.

I hate that stuff, its a pig of a solvent generally speaking, and annoyingly high boiling, although its useful for certain applications still. But I still hate it:p
Was kinda assuming that since he had ether at his disposal he at least was not in the jungle, ordering peasants to tread vats of coca leaf, petrol and lime.
Because SURELY nobody actually would resort to using PETROL for a lab solvent!!!!!!


And I didn't mean using Ph3P to stabilize the ether, just to go twat any peroxides needing gotten rid of. How much BHT or BHA should one use to stabilize EtOEt, THF and diisopropyl ether thats not intended (in the case of diethyl or diisopropyl ether) for potentially drinking. I could do with buying some BHT when I get round to it and have money to spare, because the two main sources of my ether, are one in eastern europe and the ether she supplies me with, likewise THF are uninhibited, and of course so is that made via Williamson synthesis or the preferable (to me) dehydration-autocondensation of EtOH using 95% sulfuric acid at about 115-120'C, dripping in the alcohol slowly and distilling the diethyl ether formed off as it is born.


Peroxidation is retarded in wet ethers? how much so?

*uuuhhh Hiiighhh...Eeeeyymm chlooroform peroxide....look at my tellurium-tellurium bridge, eyye go boom when silly billys open bottles of me when I'm sleeping in the screw thrradddss*

(retarded peroxide formation) *squadron of ethylidine peroxide molecules marching in formation. HAALT...* *one of them is walking backwards carrying a plastic spoon instead of it's rifle*
 
Oh yeah, "kerosene" is awful in terms of a practical solvent. Both because the average kerosene/white gas is unusually high boiling, and also due to a total lack of consistency. Petroleum ether 60-80C is about as high-boiling as I would want to use on a regular basis - or heptane, bp. 98C - Bestine is really the better choice over mystery kerosene. Stoddard solvent / "mineral spirits" and the heavier grades of kero are fucking worthless as volatile solvents, smelly and greasy and ugh. Sometimes dyed too.

The ether I use comes with a couple parts per million BHT added. It's the standard ACS anhydrous grade in 18 liter tins and I have never had any issues with peroxidation. Presumably any antioxdant added to BHT will help. On paper even THC or CBD will be fine... hydroquinone for the less discering person :)

Water inhibiting peroxide formation is an old wives' tale I heard somewhere... I think the trace metal ions from tap water do the trick. Certainly it will also inhibit the polymer formation.
 
Since metal ions are possibly the responsible party (is it actually possible to have a party thats responsible with a load of ether around?...the mother of the last girl didn't seem to think so and SHE was happy enough taking kids on a trip to buy phet base, providing 14 yo girls with tables stacked high with vodka, cider and beer and having them drop pills snort yopo and make out with...people=D) then its also not impossible those cans of ether were taking advantage of the metal in the cans themselves.

I will however, unless you know where I can buy it by the pound, forgo on adding THC to my ether as a stabilizer. Because I'd end up drinking it all and having nothing for practising the art of chemistry. That said, I wouldn't turn my nose up at the chemical houses if they decided to bring out a line of THC-CBD-stabilized diethyl or diisopropyl ether. Hell even something undrinkable like THF (not that I've tried, not that I am going to either) could benefit from some THC, if one envisions something akin to dipped smokes ala PCP.
 
I think you only need ppm quantities of THC or other antioxidants, not psychoactive amounts ;)
 
All the same, any THC that *I* would put in ether, is to either purify it, or more likely, after heating, dissolved subsequently in ether, and poured into a shot glass.

Never tried drinking diethyl/diisopropyl ether with THC in it, but the thought is quite tempting. Alcohol-free green dragon would be lovely:)
 
I'm not using any of these things specifically FOR my interest in chemistry or THC (albeit those things are both amazing and exciting). I'm also trying to reduce the harm of corrosive and stinky batches of sherm (that will either way be smoked) by exfoliating it somehow into some form of cleaner and not so deadly angel dust without seeming like some street punk who's only done dxm acid base extractions, and whom might be in some people's eyes not worthy of such information that would really be just helpful and more easily understandable if it was done in a "for dummies" type of way... Basically what I'm trying to say is... I didn't understand your chemistry jargon and I'm not even sure if you understood what I was asking... I just want to find a way to turn sherm into some form of angel dust and not have it be more complicated then a dxm extraction... I mean surely this MUST be possible... I've seen parsley dipped wetsticks on rare occasion crystallize just sitting in a plastic bag... I'm sure those conditions can be repeated more efficiently in an actual extraction somehow... that's simple? PM me if it makes ya feel better... Just if you can... please do help... this problem is getting tiresome... :) Thanks...
 
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Okay so it would work in the same way if done the same way? my question with that is with a syrup extraction you can clearly see the syrup and solvent layers seperated how could you do that with layers that I would think would look the same...
 
If its in pet ether/kerosene, then pull it with diisopropyl ether, which can be carefully distilled under a current of nitrogen or argon as welding gas disposable tanks, from some starting fluids, some are diethyl ether/heptane mixture and a fractional quantity of high boiling cylinder lube, some are a mix of diethyl ether, diisopropyl ether, and acetone, heptane, with traces of cylinder lube.


Diisopropyl ether needs testing for peroxides before distillation, repeatedly during it, unless tested first using potassium iodide/starch paper, then testing a few drops repeatedly during distillation under inert gas, then most certainly testing after. If storing it, testing the product post-fractional distillation, of course keeping the ether and heptane and re-fractionally distilling said products.


Test ether for peroxides yearly, THF 6 monthly minimum, and test diisopropyl ether every 3 months minimum, test more often if possible. THF likes to peroxidize, diisopropyl ether is a peroxidation fucking demon in liquid boom-loving form.
 
That seems tricky. I was thinking that it can't be much more complicated then a dex extraction because of how it crystalizes even just when the wetsticks dry.

If one was to just do an acid/base extraction how would one differentiate the sherm/other solvent layers? And would one use naptha?
 
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A seperatory funnel. This is a pear-shaped flask of a sort, with the narrower end at the bottom, progressively narrowing, until a stopcock with a hole in a ring-shaped section fitting sideways at the juncture of a mid lengthish length of glass tube, and a ground glass joint for a stopper at the top (so bilayers can be mixed)

Then when the stopcock is turned to the position that the hole within the centerpiece is in the open position, vertical with respect to the tube, leading to the exposure, when turned, of the open hole on the vertical axis rather than the closed position (horizontal with respect to tube/flask part) and thus allows liquid to drain slowly through the small hole, and as the flaskish bit narrows, it thus allows the part of a bilayer insoluble in the other at the bottom to be drained off first. With H2O and the likes of toluene, benzene, xylene, pet.ether (high grade light naphtha), other alkanes, aromatics its at the top, same with diethyl ether. With chloroform, dichloromethane and many other dense solvents, plus many other dense, heavy nonpolars, its at the bottom. One looks for a difference in appearance, as ideally the two solvents will have a different refractive index to each other.
 
Basically all you have to do to know which solvent is at the top and which at the bottom is compare their densities, the more dense liquid is at the bottom.
 
So mix the starting ”fluid” with the new solvent? maybe 50/50 equal amounts or no... just shake it or? Then let it settle... then separate in funnel... then evaporate? is that all? If someone in the know could explain it step by step in a private message? Layman’s terms... big time... by the way I have tried just plain evaporating starting fluid.. for some reason the ”alkaloid” evaporates with the fluid... sort of like e-nicotine juice, not sure why but need to avoid that as well?
 
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Wow, 5 years later! Sorry I'm not qualified to answer your question, but it's impressive to me that you started this thread 5 years ago and are just now getting back to it.
 
Short answer: there isn’t an easy, non-complicated way to go about what you’re discussing. Sounds like PCP freebase and you’d need to form it into a dry salt for best storage purposes. Short of that, I would say it will survive best in a sodium borosilicate glass jar kept in a cool, dark place.

Long answer: ok, here goes…
for some reason the ”alkaloid” evaporates with the fluid...
It’s because “sherm” is freebase PCP not in a crystal/salted form. I’m not sure how that factors into your experience of seeing dippers crystallize unless those dippers were dipped in something other than PCP… typically, drugs in their freebase form are oils, but if bonded to an acid they’re salts. This is true for the majority of alkaloids out there (nitrogen-bearing chemicals with physiological effects on humans).

They’re also not very stable in base form, nor are they water-soluble. If you bond a freebase drug to an acid, it will form a water-soluble salt that often takes a crystalline form, but could also be more of a powder depending on the drug and the acid and a few other factors.

If you bond PCP to hydrochloric acid, for example, you get phencyclidine hydrochloride (PCP.HCl), which has much better shelf-life. Hydrochloric acid is sometimes called Muriatic acid and is sold in many places as it’s useful for cleaning driveways, pools, stone, cement, and shit like that. I guess you could alternatively form PCP.citrate using citric acid and/or PCP.ascorbate with ascorbic acid (read: Vitamin C). That would have the added bonus of making things a bit citrus-y, which let’s face it, anything smells better than fresh Sherm. That shit is pure wretchedness, but boy are the effects beautiful and pronounced. @Gnomelad knows what I’m talking about, but if you’re reading this and you’ve never smoked PCP, you might be missing out on something awesome… however, mileage varies.
I'm also trying to reduce the harm of corrosive and stinky batches of sherm (that will either way be smoked) by exfoliating it somehow into some form of cleaner and not so deadly angel dust
Ok so exfoliating refers to skin and the shedding of topmost dermal layers and shit, right? And it’s not that you’re using some kind of “cleaner” so much as you’re talking about a non-polar solvent. Some things are polar, others non-polar. Water is polar because each molecule has a positively charged side (by the two hydrogen electrons, H₂) and a negatively charged side (by the lonesome oxygen accepting the two electrons, O; together being H₂O). It’s for this reason that water conducts electricity. Each molecule is like a miniature battery with a negative and a positive end…

Meanwhile oils are generally non-polar, and that makes sense, right? After all: oil will float on water, and when mixed they separate back out rapidly upon standing. Think of Italian dressing for a moment wherein oil is on top and vinegar (5% acetic acid + 95% water) is on the bottom and the bottle needs shaking to mix before you pour it.

Ok so then chemicals that have an amine, NH₃—which comes from the word “ammonia” btw—have the aforementioned property of being able to bond with acids to form corresponding salts that are water-soluble. They are otherwise oil-(non-polar)-soluble. And then they can lose this acid molecule and return back to being a freebase alkaloid once more. Chemists exploit this property to shed both polar + non-polar impurities during an acid/base extraction.
without seeming like some street punk who's only done dxm acid base extractions, and whom might be in some people's eyes not worthy of such information that would really be just helpful and more easily understandable if it was done in a "for dummies" type of way...
Come on, man, no one is gonna take you by the hand and write up a walkthrough for you to assist in your quest to preserve your stash of PCP dippers, especially when you can easily find a tutorial on how to perform a proper A/B extraction and form that Sherm into Angel Dust.
Basically what I'm trying to say is... I didn't understand your chemistry jargon
You’re gonna have to do some of the work here, you know? No one is gonna spoon-feed this to you the way you’d like. But many things in life worth doing take hard work and determination. Look up the chemistry jargon you didn’t understand.
and I'm not even sure if you understood what I was asking...
(It’s the other way around.)
I just want to find a way to turn sherm into some form of angel dust and not have it be more complicated then a dxm extraction...
Sure, and I just want to be able to walk into the nearest pub and buy myself a round of blotter acid (make it a double) and 150 mg of molly with a side order to-go of two Xanny bars + an 8-ball of crystal meth, s’il vous plaît.

It’s really not complicated, but you’ve got to check your expectations a bit here. Clandestine chemistry lab work is a lot harder than Univeristy-or-industry-equipped lab work, but it isn’t impossible to accomplish some of the moves you’d need to do. You just have to adopt a more “can-do” attitude, I think.
I mean surely this MUST be possible...
MUST it?
I've seen parsley dipped wetsticks on rare occasion crystallize just sitting in a plastic bag... I'm sure those conditions can be repeated more efficiently in an actual extraction somehow... that's simple?
Depends on whom you ask.
PM me if it makes ya feel better...
It doesn’t; I‘m here to share knowledge and perspective, and to show support and hopefully morale for those among us bravely demonstrating civil disobedience over the subject of drug prohibition.
Just if you can... please do help... this problem is getting tiresome... :) Thanks...
Well… just do learn this time around. You’re picking up on a thread after a five-year hiatus, you know. Makes it ironic that you’re complaining the problem is getting tiresome. You’re the one responsible for learning this stuff, ya know… either way, good luck ;)
 
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