Author Topic: Short Question Thread 2.0  (Read 5709 times)

Flight

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Re: Short Question Thread 2.0
« Reply #400 on: May 26, 2013, 01:30:21 AM »
Teahead,

"Phenol, tin, colloidal stannate, organophosphonates, acetanilide, nitrate, benzoic acid and tetrapotassium diphosphate have all been used as H2O2 stabilisers!"  Quoted from SM. 

antibody2

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Re: Short Question Thread 2.0
« Reply #401 on: May 27, 2013, 02:35:54 AM »
Seems like peracid isn't used as much as the performic by the old apiary heads.

btw anyone know if the dill seed oil is worth fooling with? maybe buy up a fat stash of dill for the ol' steam treat? or at that point I could just go with some parsley seed. I suppose origins are important. That MMDA thread is buzzing with good info.

Performic IS a Peracid rxn, ie formic acid is an acid. Although other acids such as GAA may also be used

Dill seed oil is a good source of dill apiol, which will lead to DMMDA2 not MMDA
A better source of dill apiole is had by contacting producers of Carvone (the major constituent of Dill seed oil) and asking them what they do with the residue, this often contains 90+% of dill apiole and is very inexpensive.

Parsley oil is a good source of apiole and myristicin, but requires a long tedious fractional distillation.

Flight

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Re: Short Question Thread 2.0
« Reply #402 on: May 27, 2013, 11:24:33 PM »
It looks like you maybe confused Teahead.  They are both peracids and include H2O2, one is made from acetic and the other with formic.

Flight

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Re: Short Question Thread 2.0
« Reply #403 on: June 04, 2013, 07:00:10 PM »
When running Methyl Man's AL/Hg in a 2000ml flask is a 3in stir bar an absolute must.  The only stir bar available is 1in.  A larger one has been ordered, but was hoping to get started now.

Thanks,
Flight

Wizard X

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Re: Short Question Thread 2.0
« Reply #404 on: June 06, 2013, 02:20:16 AM »
When running Methyl Man's AL/Hg in a 2000ml flask is a 3in stir bar an absolute must.  The only stir bar available is 1in.  A larger one has been ordered, but was hoping to get started now.

Thanks,
Flight

Alexander Shulgin, DIDN'T use a stirring bar in his "in a 2 L wide mouth Erlenmeyer flask". http://www.erowid.org/library/books_online/pihkal/pihkal109.shtml

To 40 g of thin aluminum foil cut in 1 inch squares (in a 2 L wide mouth Erlenmeyer flask) there was added 1400 mL H2O containing 1 g mercuric chloride. Amalgamation was allowed to proceed until there was the evolution of fine bubbles, the formation of a light grey precipitate, and the appearance of occasional silvery spots on the surface of the aluminum. This takes between 15 and 30 min depending on the freshness of the surfaces, the temperature of the H2O, and the thickness of the aluminum foil. (Aluminum foil thickness varies from country to country.) The H2O was removed by decantation, and the aluminum was washed with 2x1400 mL of fresh H2O. The residual H2O from the final washing was removed as thoroughly as possible by shaking, and there was added, in succession and with swirling, 60 g methylamine hydrochloride dissolved in 60 mL warm H2O, 180 mL IPA, 145 mL 25% NaOH, 53 g 3,4-methylenedioxyphenylacetone, and finally 350 mL IPA. If the available form of methylamine is the aqueous solution of the free base, the following sequence can be substituted: add, in succession, 76 mL 40% aqueous methylamine, 180 mL IPA, a suspension of 50 g NaCl in 140 mL H2O that contains 25 mL 25% NaOH, 53 g 3,4-methylenedioxyphenylacetone, and finally 350 mL IPA. The exothermic reaction was kept below 60 ° C with occasional immersion into cold water and, when it was thermally stable, it was allowed to stand until it had returned to room temperature with all the insolubles settled to the bottom as a grey sludge. The clear yellow overhead was decanted and the sludge removed by filtration and washed with MeOH. The combined decantation, mother liquors and washes, were stripped of solvent under vacuum, the residue suspended in 2400 ml of H2O, and sufficient HCl added to make the phase distinctly acidic. This was then washed with 3x75 mL CH2Cl2, made basic with 25% NaOH, and extracted with 3x100 mL of CH2Cl2. After removal of the solvent from the combined extracts, there remained 55 g of an amber oil which was distilled at 100-110 ° C at 0.4 mm/Hg producing 41 g of an off-white liquid. This was dissolved in 200 mL IPA, neutralized with about 17 mL of concentrated HCl, and then treated with 400 mL anhydrous Et2O. After filtering off the white crystals, washing with an IPA/Et2O mixture, (2:1), with Et2O, and final air drying, there was obtained 42.0 g of 3,4-methylenedioxy-N-methylamphetamine (MDMA) as a fine white crystal. The actual form that the final salt takes depends upon the temperature and concentration at the moment of the initial crystallization. It can be anhydrous, or it can be any of several hydrated forms. Only the anhydrous form has a sharp mp; the published reports describe all possible one degree melting point values over the range from 148-153 ° C. The variously hydrated polymorphs have distinct infrared spectra, but have broad mps that depend on the rate of heating.
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fishinabottle

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Re: Short Question Thread 2.0
« Reply #405 on: June 07, 2013, 08:39:57 PM »
When running Methyl Man's AL/Hg in a 2000ml flask is a 3in stir bar an absolute must.  The only stir bar available is 1in.  A larger one has been ordered, but was hoping to get started now.

Thanks,
Flight

A 1" stirbar is ok with a 2l flask, with a bigger one you must be asolutely sure that your stirplate will pull it through a highly viscous liquid, what is not to expect if you dont have a heavy duty model.

Stirbar size is a little bit like penis size, or it was at least with everybody claiming to have a bigger one. Whats nonsense of course, as real men in realworld use overhead stirrers for tasks like this.
Once you had one in use you wont go back. Same with a big penis btw.  :o

/ORG
« Last Edit: June 07, 2013, 08:41:47 PM by fishinabottle »

Flight

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Re: Short Question Thread 2.0
« Reply #406 on: June 07, 2013, 10:31:46 PM »
Quote
A 1" stirbar is ok with a 2l flask, with a bigger one you must be asolutely sure that your stirplate will pull it through a highly viscous liquid, what is not to expect if you dont have a heavy duty model.

Stirbar size is a little bit like penis size, or it was at least with everybody claiming to have a bigger one. Whats nonsense of course, as real men in realworld use overhead stirrers for tasks like this.
Once you had one in use you wont go back. Same with a big penis btw.  :o

/ORG

Can any type of agitator be used for a DIY over head stirrer? Like the type that is placed on a screw driver to mix concrete or does it have to be made of a specific material?

Thanks,
Flight

no1uno

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Re: Short Question Thread 2.0
« Reply #407 on: June 07, 2013, 11:01:15 PM »
Depends strongly how easily it can be stabilized or you are going to chip/break the neck of your flask, if it is going to be used with anything flammable, something spark-proof would be useful, or a belt-drive could be used to run it from a shielded position (like Parr uses).  Much easier to find a spark-free drill, than fucking around - and a paint mixer is essentially what you are going to be running.
« Last Edit: June 07, 2013, 11:03:27 PM by no1uno »
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Wizard X

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Re: Short Question Thread 2.0
« Reply #408 on: June 07, 2013, 11:21:51 PM »
Make your own rubber bung stirrer. See picture...
Albert Einstein - "Great ideas often receive violent opposition from mediocre minds."

fishinabottle

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Re: Short Question Thread 2.0
« Reply #409 on: June 08, 2013, 10:47:42 AM »
Quote
A 1" stirbar is ok with a 2l flask, with a bigger one you must be absolutely sure that your stirplate will pull it through a highly viscous liquid, what is not to expect if you dont have a heavy duty model.

Stirrbar size is a little bit like penis size, or it was at least with everybody claiming to have a bigger one. Whats nonsense of course, as real men in realworld use overhead stirrers for tasks like this.
Once you had one in use you wont go back. Same with a big penis btw.  :o

/ORG

Can any type of agitator be used for a DIY over head stirrer? Like the type that is placed on a screw driver to mix concrete or does it have to be made of a specific material?

Thanks,
Flight



This now is true for the Al/Hg and for Fe/HCl reactions, it may or may not be true for other reactions!

A stainless steel tube or rod can be used as shaft and 3mm PTFE can be cut for blades. Half-moon shaped blades running 0,5cm, not more, above the flasks bottom. in a 2l flask 7 to 8cm wide is enough, stirrer speed wont exceed 400rpm at most anyways.
Some wellknown chinese lab-discounter sells stirrer bearings at less then 20$ and the stirrblades and shafts are rather cheap too - I made most of my own things myself but looking back I would just buy it.
If you want to improvise you need:

- A motor with rpm's regulated
as most practical are known motors from sewing machines. They have the torque and a nice footregulator. I would not worry to much about explosions - good ventilation is a must anyways or you get deadsick from methylamine poisoning. Famous PARR was when I looked the last time still selling their shakers (hydrogen! pressure!...) with cheapo motors - explosion prove costs extra. So lets not get more catholic then the pope here....
 
- a flexile connection of motor to stirshaft
Thats just a rod of some elastic plastic, something sturdy, the GFK rods for gardening for example. You need just 15 to 20cm. Red rubbertubing to connect this, I show you a picture.

Dont use the infamous vacuum rubber tube connector as shown in many if not most older chemistry books. Say just some of such tubing and thats it! You are heading into disaster with this in a reaction which gets hard to stirr.
The reason is that sometimes something tries to block the blade and then the weakest part of the contraption gives way. And thats the tubing. It will twist like a corkscrew and in doing so it will shorten but with an incredible force. It will rip your setup into pieces before you can spell "SHIT!" shattering your flask if you are unlucky.
Using the plastic rod as described the PTFE blade will bend and nothing bad happens, a hiccup nothing more


- A rod. SS tube 10x1mm. Take a hammer, flatten one end on 10cm length and drill a hole. SS for the screw to fix the blade which must pivot to get through the neck.

- The blade from PTFE 3mm thick, no other affordable plastic can be used, thats not expensive, though for making two yourself you can buy one in china.

- stirrer bearing to lead the shaft through the neck and stabilize it.
Thats tricky to make, buy it! Or use the suggestion from the post above but you must take two rubber stoppers fixed ass to ass so the earing is long enough to take the load. Also dont inser one glasstube (which will break, as glass doesnt bend, but use two shorter glasstube from top and from bottom and some space between. The glass must be completely in the rubber, no peeking out.

pic 1: flexible connection
pic 2: SS shaft and PTFE blade after some iron/HCl. Oxalic acid cleans it.

/ORG


« Last Edit: June 08, 2013, 10:51:40 AM by fishinabottle »

fishinabottle

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reduction under a flow of hydrogen
« Reply #410 on: June 08, 2013, 01:26:15 PM »
Many preparations of catalysts call for a redcution under a flow of hydrogen at elevated temperatures, usually 350 to 550 or more °C.

Doing this without a well equipped laboratory seems a bit a challenge, so:

Does anybody know of a procedure to reduce metal(oxides), load it with hydrogen, otherwise? Without the gasflow at high temperatures? Electrolytically? Magick?
Alternativly, knows somebody a working setup for the hydrogen reduction, with specifications for material used and not just for 2 grams of catalyst. 50 to 100g to make this interesting.

But of course the first would be much preferred  ;)

regards
/ORG

java

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Re: Short Question Thread 2.0
« Reply #411 on: June 08, 2013, 04:40:51 PM »
Reference Information





Hydrodehalogenation of Aromatic Halogens Using Sodium Borohydride and Palladium under Ambient Conditions
Zach M. Rousslang, Alyssa Russo
Pacific University Oregon
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newbiechem

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Re: Short Question Thread 2.0
« Reply #412 on: June 11, 2013, 12:01:07 AM »
please....

whats the role that alchool (etano) plays on the oximization of a aldehyde?

can one exchange etanol for methanol on same rates to form the aldoxime?

thanks for the help

peace

lugh

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Re: Short Question Thread 2.0
« Reply #413 on: June 11, 2013, 01:39:52 AM »
A quote from the hydroxylamine article in Thorpe's Dictionary of Applied Chemistry

It is used for preparing oximes of aldehydes and ketones. Aldoximes are usually prepared by adding the aldehyde (1 mol.) to an aqueous solution of hydroxylamine hydrochloride (1 mol.) and sodium carbonate (1.5 mol.). Aqueous alcohol is used for water-insoluble aldehydes. Ketoximes are somewhat more difficult and are usually prepared by heating the calculated quantity of ketone, hydroxylamine hydrochloride and sodium acetate in aqueous or alcoholic solution 1-2 hours on a water bath. Also by heating the ketone dissolved with alcohol, and hydroxylamine hydrochloride in a sealed tube for 8-10 hours at 160-180° (I. Schmidt Houben, Die Methoden der organischen Chemie,'' 3 Aufl. 1930, 584)

that may clarify the matter  ;)  Thorpes Dictionary of Applied Chemistry is available from Gallica:

http://gallica.bnf.fr/?&lang=EN

and Houben-Weyl is available from Book Finder:

http://en.bookfi.org/s/?q=Houben&t=0

like may other textbooks  ;D  The end results from the effort applied  8)
« Last Edit: June 11, 2013, 02:41:49 AM by lugh »
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carl_nnabis

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Re: Short Question Thread 2.0
« Reply #414 on: June 11, 2013, 06:18:27 PM »
Ok, well, ive got some sodium metal stored under paraffin oil, now ive looked onto it after several weeks of storage, and i discovered it all got red and somehow slimy(the oil), so my question is, what could have happened there?
The sodium was rinsed clean with pet-ether and put into some for further storage.
Seems fine now, but can somebody explain why this has occured?
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