Author Topic: Questions for Lestat: Lestat's Lab  (Read 2210 times)

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Offline Lestat

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Re: Questions for Lestat: Lestat's Lab
« Reply #90 on: April 12, 2017, 10:46:02 AM »
Fractional distillation of a tertiary mixture (ethanol, H2O and n-pentane)



Flask on the right contains the mixture to be distilled, with a distillation adapter (reversed in configuration, in order to be able to use a distillation bend that hadn't got a vacuum takeoff barb on it which really is not needed in this application, the boiling point of n-pentane is just 35.9 'C whilst that of ethyl alcohol is just over 70 'C so this is a simple fractional distillation of two liquids of opposite polarity, intermixed with water, diluting the alcohol, next, is the condenser, a short, highly efficient design called a Dimroth condenser, which is pretty much, design-wise, a reversed graham condenser, in a graham, the cooled liquid runs through the spiral column in the center which is usually, in a graham condenser, a single twisted spiral, whilst a Dimroth has a helix, in the graham the thing being distilled goes through the center spiral, in a dimroth its the reverse, and it goes through the outside, whilst the coolant line feeds through the center helix. The graham design suffers from the fact that the bore is narrow and can easily get clogged, plus they are not much cop for reflux since the narrow, twisty bore traps the distillate too easily and if they get choked with solids that can result in a catastrophic pressure buildup. I have one, I rarely use it. A Dimroth condenser on the other hand doesn't suffer from this since the coolant is what goes through the inner coil, which is of a wide surface area, mine has a little drip-tip on the bottom of the helix too, to assist refluxes, in the upright configuration, so condensate can drip back off it into the boiling flask. The Dimroth condenser design is compact, and highly efficient, suffering from very little drawbacks. Normally quite pricy, but I got mine on ebay, 24/40 joint tapers, for a less than £20, somewhere around £14 IIRC, which is an absolute STEAL of a bargain, there were quite a few others watching that auction and I sniped the bid at the last few seconds with an automated program for it. Real bargain, probably my favourite out of all my condensers (I've quite a few Liebigs, a simple jacketed straight bore design, an Alihnn, which has a straight outer jacket and multiple bulbs meeting at a wasp-waist like interface as the inner bore, a Graham spiral coil condenser, and the Dimroth. Next I am going to be buying myself a dry ice/liquid nitrogen condenser (cold finger) for condensing and refluxing cryogenic gases.


Simple air condenser setup, since my water pump is currently being employed for keeping some iodine monochloride cold, and it has to be, because ICl is both dangerous, volatile and highly reactive. Plus uses expensive iodine to make it, so I can't just shift the pump elsewhere. Dual feed air pump, spliced both feeds together for greater flow.


Flask on the left, now has a fresh ice-salt-water-acetone-ethylene glycol freezing mixture in it, the plastic bag fragment is just because I made a bunch of ice in bulk blocks by freezing large sandwich bags full of water, tightly tied up and stuffed in the freezer. Just temporarily, had to move the distillation setup outside, because my old man needs the pans I'm using for hot water and freezing mixture baths to cook dinner. From the behaviour of the solvent mixture, most of the pentane has been distilled off, anyway, and the receiver flask has been briefly dunked in the freezing bath to stop the distillation (no real risk of thermal shock since its borosilicate glass, and pentane has such a low BP that it didn't have to get very much more than warm to begin with) whilst the receiver is still in the freezing mixture so I don't lose the pentane. Which will be redistilled from a portion of drying agent, such as first anhydrous epsom salts then from something irreversible, like lithium metal once its dry enough that there will be no flames as this is done. Li will react with the water to form lithium hydroxide (which needless to say, will be saved for later electrolysis and recovery of the lithium once fused into a melt) whilst the highly unreactive, saturated aliphatic hydrocarbons are extremely resistant to being protonated or deprotonated to carbocations/carbanions respectively, and it would take a base MUCH stronger than LiOH to deprotonate aliphatc saturated linear hydrocarbons, I'm not even sure sodium hydride would do it (CBF crunching the numbers, since its not something I'm about to need to do anyway)

And then once dried, redistilled and fractionated again to cut out any remaining water or ethanol; and stored until it is wanted for use.                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                       
« Last Edit: April 12, 2017, 11:20:27 AM by Lestat »
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Offline Lestat

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Re: Questions for Lestat: Lestat's Lab
« Reply #91 on: April 12, 2017, 02:45:59 PM »
And once that is done, I'll be doing a synthesis of chloroform, CHCl3, via the haloform reaction. And possibly also of 1,2-dichloroethane using concentrated hydrochloric acid to chlorinate ethylene glycol, assisted by means of ZnCl2 as a lewis acid. I'll first have to prepare the zinc chloride though. Might just do the ethylene dichloride since I have plenty ethylene glycol and its a lot cheaper in larger quantities compared to acetone, which I'd oxidatively chlorinate to give chloroform.
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Re: Questions for Lestat: Lestat's Lab
« Reply #92 on: April 14, 2017, 12:30:58 PM »
Finally, I hope. found a host for my iodine monochloride video that didn't want verification by phone number (sorry, not getting anything that can identify me :P)

IClfinal.mp4 its a download rather than a direct link, about 86 total)

This installs a toolbar, just delete it after asap, was the only place that didn't ask for ID of some sort.
Just thought I'd warn you. File is .MP4, has had the metadata removed, so windows media player won't play it. VLC media player is free and it doesn't have any issues.

Notes-If following my synthesis, do not retain the no-hole stopper whilst passing Cl2 or other gases through the drying agent/iodine, otherwise pressure WILL build up and force a joint apart, whichever is weakest, resulting in the venting of Cl2 through the system to the atmosphere. This was placed in there to avoid anything volatile evaporating, such as the iodine, and escaping. It seems however, save to SLOWLY pass Cl2 through the system even so, given it reacts with the iodine to form a liquid, or in the case of excess Cl2, either through I2 or ICl, to form the trichloride, ICl3. This can be done by adding HCl and hypochlorite via large syringe, such as a 60ml oral/enteral medical feeding syringe without a needle attached to a short length of rubber hose, using a distillation adapter to connect the Cl2 generator to the liebig condenser, and a short length of rubber hose, serving to mate the syringe (clamped whilst attaching the syringe and during its removal to refill), during the synthesis itself however, a stopper with one hole and a long piece of glass tubing, attached first to a suckback trap (I superglued a one-way valve and seal to a medicine bottle cap, just to prevent water suckback into the iodine monochloride accumulating in the receiver, this would be disastrous, certainly damned unpleasant, since it would hydrolyze the product  back to iodine and chlorine gas, and a little would produce a lot of toxic gas.)

A respirator with a cartridge suited to acid gases and halogens is REQUIRED, ICl is highly toxic, more so than chlorine gas.

Use teflon and if grease is to be used, use a perfluorocarbon grease, since ICl is a STRONG oxidizer and will reduce the likes of dow-corning high-vacuum grease, or petroleum jelly to the consistency of set cement, so wrap stoppers in heavy layers of teflon tape and perfluorocarbon grease both under and over them, likewise any glass to glass joints need such treatment because should you try and unstick a jammed stopper and get this stuff on you, I shudder to even contemplate what it would do to flesh. Don't use metal vessels to transfer or store it, it will eat through them. It does not attack glass, but DOES attack plsatics, viciously so, also the vapor can slowly permeate through plastics.  Outlet gases and vapors should be led through a suckback trap, and then into a solution of saturated sodium, potassium carbonate etc. AFAIK it decomposes in carbonate, although not bicarbonate, to iodates) hydrolytic decomposition is violent and rapid. i've only added drops at a time to water to test how quick this occurs and it is instantaneous, a little puff of green Cl2 gas given off and iodine sinking to the bottom of the water. A large quantity of this compound would, most certainly, result in a correspondingly large release of chlorine gas, and quickly. Not desirable, not pleasant, not safe.

Needless to say, you don't want this happening in your lungs or eyes, WEAR A FUCKING MASK AND FACE SHIELD, with goggles underneath the shield, and long, elbow-length gloves. ICl is HIGHLY TOXIC and can also be ABSORBED THROUGH THE SKIN, affecting the kidneys as well as the lungs. No, it wouldn't make a good kitchen spice  :green:

I can't stress enough-FACE SHIELD covering FULL FACE, the more the merrier. You wouldn't get chance to react it this got in your eyes, chances are instant blindness would be the result. Not to mention it would hurt like fuck. Oh, and turn to acid while it broke down in the tear fluid. On skin, SEVERE burns, near instantly. Chances are they would be deep burns, up to third degree. Easy synthesis, lots of safety precautions needed and great care taken with the procedure.

Some notes as to the video-second little part of the sections spliced together got repeated, ignore that, video looks good.

I said during one early part that the medical air pump was being used to drive the Cl2, this was a momentary lapse of narration, its argon from a tank being used for this, the medical air pump is in fact plugged into the liebig condenser with the drying agent (closest to the right-hand flask) to pre-cool the Cl2 gas before it enters the water-cooled condenser packed with I2)

The beginning of the rxn can be seen when the orange color forms, this is where the chlorine first meets the iodine, and a little iodine TRIchloride forms (a reversible rxn) the monochloride is a dark, bromine-like liquid of low melting point (two melting points actually depending on whether its alpha- or beta-ICl formed, the  alpha crystal form gives long needle-like crystals when solidified, the beta form gives rhombohedral plates). Oddly, it can supercool from the looks of it, remaining liquid even when immersed in cooling baths of things like ice-ethylene glycol or diethylene glycol, acetone and methylated spirits with a little water and salting the ice, this gives a sub-zero temperature, yet nevertheless, I have personally seen ICl remain liquid despite this, and despite it being colder than its melting point.

To contain ICl, keep it out of light for prolonged periods, brief exposure such as to open a bottle and use some of the reagent is alright, its air-sensitive and moisture sensitive (atmospheric water content included), preferably backfill the bottle containing the ICl with argon or nitrogen for storage, wrap the screw-thread of the bottle with teflon tape, and use a bottle with a teflon cap and a resistant seal. In such a bottle, the ICl I made, I still have, in good condition without any noticeable hydrolysis.

ICl3 on the other hand, should be stored under an atmosphere of dry chlorine gas, for it is, I believe, unstable under an air atmosphere and I am not entirely sure about under inert gas. Excess chlorine should be used as the atmosphere of the bottle in order to prevent decomposition. Not done anything myself with ICl3 yet. DO NOT let it contact METAL POWDERS, risk of spontaneous ignition, and certainly one small flame and it'll burn instantly and intensely) bulk metals, E.g iron bar, etc. etc. would just corrode rather than burst into flames. Phosphorus (red) is hypergolic with ICl, the very moment the two contact, such as one drop falling on red phosphorus powder, the RP instantly ignites. Haven't tried it on white phosphorus but its even more reactive than the red allotrope, the reason I haven't, is that whilst I have most of whats left of 2kg red phosphorus on my lab reagent stockroom, I have only a small sample of white phosphorus, and I don't intend on just burning it for no gain. There isn't the slightest doubt that it would burst into flames, since ICl is a strong oxidizer.

Oh and don't use plastic keck clips, because even heavily  wrapped in teflon tape, and greased to fuck, then wrapped again, they without exception, disintegrate just from the traces of ICl that manage to make it out of the glass fittings. This happens quickly indeed, You'd be lucky to have one last a full hour before disintegrating or cracking straight through, and whilst I've not tried it, the only solvents I'd trust, are highly inert ones, such as fluorocarbons, dichloromethane, carbon tetrachloride, or possibly chloroform. ICl eats things. even the lawn around the table the apparatus is set up on is now bleached pale yellowish white (over time). Likewise don't do this in the rain, you really do not want ICl or ICl3 getting in contact with water.

And where my voice changes, those are just momets when I need to wear a gas mask,
If intending to produce solely ICl rather than ICl3, there is a little trick, that being to use excess I2 in the iodine column, and any ICl3 (yellow-orangey solid) formed can be left overnight, the excess Cl2 or/and ICl3 reacts with the excess iodine to reform ICl after leaving the setup overnight. Iodine isn't too cheap, especially due to the high atomic weight of iodine, so the less wasted the better, Those streaks of ICl3 in the I2 column reverted on standing overnight to give ICl once again)

In bright weather, cover the receiver pluss the I2 column with tin foil just to keep out the light and enhance stability of the monochloride.

It adds to alkenes (olefins, carbon-carbon compounds containing a C=C double bond) like for example, bromine does, forming in this case not a mono or dibromide, but a mixed iodobromide where one of the halogen atoms adds to one end of the double bond, and one to the other, this inclides substitution on a cycloalkene ring. Alexander 'sasha' Shulgin, rest his great soul, also used I found out later after making the reagent, iodine monochloride as the iodinating agent in his sytheses of DOI and 2C-I (2,5-dimethoxy-4-iodoamphetamine and 2,5-dimethoxy-4-iodophenethylamine) respectively. ICl                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                      was used .

So, enjoy, folks.                                                                                                                                                                                                                                                                                                                                                   
« Last Edit: April 14, 2017, 02:33:25 PM by Lestat »
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Offline Lestat

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Re: Questions for Lestat: Lestat's Lab
« Reply #93 on: April 26, 2017, 05:29:09 PM »
Adaptation of the mercury amalgam technique reducing agent using CuCl2 to depassivate aluminium, trial out on aliphatic ketone (C3, acetone)

http://www43.zippyshare.com/v/UAvwSBT6/file.html

Aluminium_Copper couple adaptation of Al-Hg reduction.avi
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Offline Lestat

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Re: Questions for Lestat: Lestat's Lab
« Reply #94 on: April 29, 2017, 08:39:13 PM »
For something I can't afford to use the experimental copper 'amalgam' technique on, owing to time spent in preparation, having to make almost everything from scratch...

A LOT of condenser (allihn type reflux condenser, 300mm vigreaux column in the middle with a liebig condenser attached to an air compressor at the very top...this is going to get rather toasty rather quickly)


Blue thing on the right-air compressor, model, not sure, came from a hospital, brown feed line to liebig condenser (top of the three, allihn on the bottom, cooled by an ice-water-ethylene glycol-denatured alcohol feed using a fish pond water pump, clear hose attached to upper hose barb of the allihn, attached to the two-neck, 1l round bottom flask, thermometer adapter in the other neck with thermometer in it, set to 40 'C, readying ice bath for in case the little sucker overheats and starts rising up to the level of the vigreaux column (middle of long condenser section with the indentations to assist cooling, usually used for fractional distillation, although in this case its helping shoulder the load when this reaction starts to kick off)

Stirbar in bottom of flask (homemade, by sealing a samarium-cobalt rare earth magnet in a length of borosilicate glass tubing, made a neck in it to hold the magnet then fused the other end closed using a torch and carbon tools to manipulate the molten glass (glass doesn't stick to carbon like it does to metal) then reversed the tubing after the glass had cooled and fused that end closed, cutting off the excess glass, aside from a long sharp fiber like projection that I simply burnt off with the torch)

Several liters of ice in the off-reddish pink large bowl thats supplying the coolant feed to the allihn condenser along with the coolant mixture, ice bath being readied before the reaction starts in case of overheating (separate ice bath that is, just for cooling down the flask if/when it starts to get really exothermic, although hopefully reagent addition done portionwise will avoid the exotherm getting to more heat than it takes to keep the reaction self-sustaining with its own heat as hydrogen generation begins. Although as the hotplate/mag stirrer had to be repaired and an external controller fitted to bypass the thermostat in the plate, I do need to keep a minimal level of heat
set to 'on' as the heater and magnetic stirrer share a common power feed at the moment so the stirrer won't run with the heat set to zero. Doesn't need much, just needs to be on and barely above minimum though)

One of the longest condenser setups I've ever used. I'd have added my Dimroth condenser (short, but highly efficient) as well, but spatial constraints mean I have to work here instead of the lab, because even here, the condenser is just barely below actually poking the ceiling, its about an inch to an inch and a half short of the roof.



« Last Edit: April 29, 2017, 08:43:59 PM by Lestat »
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Re: Questions for Lestat: Lestat's Lab
« Reply #95 on: April 29, 2017, 09:30:39 PM »
What sort of camera do you use? I hope I don't offend you by saying that you need a new one!
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Re: Questions for Lestat: Lestat's Lab
« Reply #96 on: April 29, 2017, 09:47:47 PM »
That shot was taken at long distance, from right the other end of the room, it had to be because of the length of the condenser setup.

And a digital camera. The make and model I keep to myself (it would be a bit self defeating to spend the time removing exif and other metadata from my pics including make, model, serial number of camera, geolocator tags if this thing has GPS (not sure if it does, but I strip out all metadata that can carry any identifying information for security reasons, and no you don't hun, why would you?)

Resolution-wise, its a 5 megapixel camera, I've had it a fair while, can't afford to buy another whilst this one works though. Not as good at longer ranges as it is at macro close-ups, at which it does alright, could barely fit that condenser tower in shot from the other end of the room though.                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                           
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Re: Questions for Lestat: Lestat's Lab
« Reply #97 on: April 29, 2017, 11:03:41 PM »
Ah, we too have a 5 megapixel camera. But we don't use it as our phone cameras are better. My phone has 8.

I remember my first phone that had a camera wasn't even 1 megapixel. It was really awful. I took a photo of some ducks once and they turned out to look like grey blobs. I pretty much didn't even bother taking photos with that phone afterwards.
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Re: Questions for Lestat: Lestat's Lab
« Reply #98 on: April 30, 2017, 01:28:26 AM »
That shot was taken at long distance, from right the other end of the room, it had to be because of the length of the condenser setup.

And a digital camera. The make and model I keep to myself (it would be a bit self defeating to spend the time removing exif and other metadata from my pics including make, model, serial number of camera, geolocator tags if this thing has GPS (not sure if it does, but I strip out all metadata that can carry any identifying information for security reasons, and no you don't hun, why would you?)

Resolution-wise, its a 5 megapixel camera, I've had it a fair while, can't afford to buy another whilst this one works though. Not as good at longer ranges as it is at macro close-ups, at which it does alright, could barely fit that condenser tower in shot from the other end of the room though.                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                                           

Your camera is fine. Try to increase your lighting level to force your camera to use a shorter shutter speed.
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Ghandi: Live as if you were to die tomorrow. Learn as if you were to live forever.

The end result of life's daily pain and suffering, trials and failures, tears and laughter, readings and listenings is an accumulation of wisdom in its purest form. (from My heart to You! Never stop learning!)

Offline Lestat

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Re: Questions for Lestat: Lestat's Lab
« Reply #99 on: April 30, 2017, 08:59:37 AM »
Thanks dirtawg. I can do that artificially with the camera.

As for phone cameras...not got one. Do have a phone, it just doesn't have a camera, its a pretty basic bare bones thing that cost about a tenner, some of my old phones did, lol I remember when they still came separately and had to be plugged in.

The thing I've got atm is a spare, that the filth didn't steal when they broke in here, fucking cocksuckers. Hope to get the bastards this time, owing to a false warrant (what was on there as the purpose of the search and what I was arrested for isn't even a crime, got a fair lot on them this time. Refusing to show ID, attempted coercion of a false confession by withholding medical treatment and food...I'm going to light a fire under their arses and gleefully watch their ballsacks roast in hell.



Its just as well that I did set up that huge condenser chain, destroying the aluminium sludge and remaining excess pieces had the thing boiling hard enough to send frothing, seething hot caustic, mercury-laden solvent froth right up the ice/salt/antifreeze/water/alcohol bath that was being circulated through the condenser and into the base of the vigreaux column. And that was with a slow, steady addition of saturated NaOH, no more than opening the thermometer inlet, taking it off for a moment, and pouring in a splash at a time.
« Last Edit: April 30, 2017, 09:04:03 AM by Lestat »
Beyond the pale. Way, way beyond the pale.

Requiescat in pacem, Wolfish, beloved of Pyraxis.

Offline Lestat

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Re: Questions for Lestat: Lestat's Lab
« Reply #100 on: July 24, 2017, 02:28:15 PM »
My very latest couple of additions to my glassware set. Two brand-spanking-new 3-way distillation adapters (still heads)

These I shall most likely baptize tonight, for the rites of purification must be performed on a certain compound, and the solvent stripped therefrom. I shall bee a very busy   :heisenberg::bee:

The lettering is a little unclear, it says '24/29', indicating the size of the ground glass joints in width and taper.


Beyond the pale. Way, way beyond the pale.

Requiescat in pacem, Wolfish, beloved of Pyraxis.

Offline Lestat

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Re: Questions for Lestat: Lestat's Lab
« Reply #101 on: October 11, 2017, 03:34:57 AM »
Currently-I've a beaker full of blackish-dark colored liquid, thats acidic as hell. My product from my latest work is in there. I've filtered off a great deal of solid-phase particulate garbate, part decanted off from the flask it was in, and the rest filtered under vacuum into my large (around 5 liter) buchner vacuum filter flask, to leave the dark liquid containing my product behind, in an extremely acidic solution, that'lll be pretty annoying to neutralize even, let alone take up to PH 11-13; since the reaction itself was perfored in glacial acetic acid as a solvent, plus a much smaller measure (100ml or so) of concentrated hydrochloric acid.

Smells totally foul. Got my full face-shield on, my elbow-length gloves on, and slowly adding sodium bicarbonate until it stops fizzing, which will tell me the acid is consumed. Then I'll start adding sodium hydroxide (lye, NaOH, caustic soda) in aqueous solution, bit by bit, electronically monitoring the PH with my digital PH monitor pen, until it starts to smell like old fish rather than acid, and IF I am really lucky, a layer of oily liquid, my product, will appear on top. This would be filtered off and saved if it does so, if not then once based satisfactorily, to the right PH, I'll either extract with toluene, then add a little bit at a time, drop by drop by drop, hydrochloric acid gas in dry isopropanol to precipitate it out from the toluene as a salt. Or else I might choose to take advantage, if extracting a smaller portion as a sample of the sae does not imediately precipitate my desired compound, then I'll extract the main body of the mixture using isopropanol, and adding lots and lots and lots of salt, warming it, until a super-saturated, and with the caustic soda, highly alkaline solution in brine is prepared, which will due to the 'salting out' effect, drive my product into the isopropanol by osmotic pressure, add a very little bit of anhydrous isopropanol solution of hydrogen chloride gas, and distill off the iPA to hopefully leave my desired product behind to be recrystallized, washed, cleaned and rendered all wuvvly and sparkly as crystals :)

Its already fizzing and bubbling and hissing and I think I might just be able to detect the first hints of 'fishy'-ness that is the hallmark of an amine in general.

Here we go. Lestat is doing what he does best, although a part of it he's never liked much. Never have enjoyed workups, in fact its always been the very least favourite aspect of chemistry of them all as far as he's concerned)

Still, needs must. What must be done must be done, that acid must be neutralized and the product taken up in solvent, back extracted and purified.
so purified it will be, until it is Lestat-issue standard. Won't be satisfied until its a work of art, not just a chemistry project.

Stinks though. Like vinegary, HCl-acid-like, copper-coin-in-sweaty-palms-smelling acrid metallic stinkyness. Yuck. still, from black slop can come glistening crystals of beauty and utility. And so they must :)

Time for Lestat to get his :heisenberg: hat on :D

Well not so much a hat as a flip up/down full-face, forehead, neck and top of the chest-protecting shield and gloves but it counts does it not :autism:
Beyond the pale. Way, way beyond the pale.

Requiescat in pacem, Wolfish, beloved of Pyraxis.

Offline Lestat

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Re: Questions for Lestat: Lestat's Lab
« Reply #102 on: October 24, 2017, 11:36:21 PM »
Said liquid, I may add, was extracted with DCM (CH2Cl2, dichoromethane, a solvent akin to choroform or to carbon tet, but with a lower boiing point, a sharper, less sweet smell than CHCl3) and the dichlor distilled off in a comfortably easy and facile distillation process after first washing with dilute (10 and 20 percent sodium hydroxide brine 4x to cleanse it if impurities, and since at the time my electric vac pump had burnt out, I couldn't vac distill the desired, produced carbonyl compound) the bisulfite adduction complex was formed, and it cleaned chemicaly. Needs but to be regenerated from this to give the ketone, using dilute mild base, such as sodium carbonate solution, extraction into DCM, drying, washing the dessicant used with a bit more DCM, them distillation off of the DCM before it is used for whatever purpose it might be desired for, amongst the many, many things a chemist can do with it directly or turn it into other things useful. Turned it from a 2 liter pot of black, stinking glacial acetic acid solvated metalliferous slurry to a little over one ounce of purified ketone, not counting the additional weight when in the form of its bisulfite addition complex. And from liquid ketone of a yellow-dark color finally to straw-pale color, tinged, and thence the adduct formed, simiarly colored and then purified by solvent washing with various sovents to a dry, crispy, crunchy dry pure-white crystalline powder, in a lovely state to look on, knowing the work that went into it, the hours spent making it and weeks spent purifying it to that just over 1 ounce of purified, super-clean carbonyl compound meticulously. I can't wait for the final use whatever I decide it to be, I have not decided yet. But there are many uses, and several ways to go about each of them. I think I know what specific use, but as of yet, am still to decide upon a method to accomplish this in the cleanest of manners.
Beyond the pale. Way, way beyond the pale.

Requiescat in pacem, Wolfish, beloved of Pyraxis.

Offline Lestat

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Re: Questions for Lestat: Lestat's Lab
« Reply #103 on: October 25, 2017, 09:19:12 AM »
Guess what lil ol' lestat just treated himself to?

The Rotavap he SOOOOO wanted, and in twice the flask capacity size too (2 liter, cost $1,050,00 )

Flask included (two liter rotavap flask), condeser, heating bath, the full fucking works to go. Oh yes oh fuck yes. One happy lestat right now. Wanted one for SO long. Never thought it'd come within my price range. And now I get twice the capacity I was after too. Fucking---niiiiiiiiihiiiice :autism: *flap*
Beyond the pale. Way, way beyond the pale.

Requiescat in pacem, Wolfish, beloved of Pyraxis.

Offline Lestat

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Re: Questions for Lestat: Lestat's Lab
« Reply #104 on: November 21, 2017, 11:54:41 AM »
Got some calcium silicide recently. Hoping I can use it for production of (eventually) phenylsilane, since while I can buy it, its something near $150 for a few tens of grams, and I want it in bulk. Well, semi-bulk, 100g at least, and it's for something I want to try involving silylation and eventual alpha-alkylation of aminoacids, using Karstedt's catalyst; and again that is REALLY expensive, its an organoplatinum complex and a few grams costs almost half a grand. And it looks like it'll be a rather complex synthesis too. Going to have me work cut out for me if I go ahead with that project. There is no WAY I am paying such prices as that for 25g (IIRC) of Karstedt's cat, readymade. So it'll be cheaper to buy platinum bullion even, and dissolve it in a suitable acid, or maybe nitrosyl chloride to produce some chloroplatinic acid and make this complicated tetramethyldivinylated organosilicon-platinum complex. But if I can manage to produce some, or buy it if I REALLY must, (its recyclable or at least regenerable, as true catalysts are, since catalysts speed up reactions but are not themselves consumed), being able to alkylate the alpha carbon of aminoacids would be one REALLY useful reaction. For example, could be the start of a really novel synthetic route to alpha-methyltryptamine, aka AMT, the entactogenic psychedelic, by alkylation of tryptophan followed by simple decarboxylation to give AMT.
Beyond the pale. Way, way beyond the pale.

Requiescat in pacem, Wolfish, beloved of Pyraxis.